EP0823120B1 - Formulation de vernis pour fils metalliques a lubrifiant interne - Google Patents

Formulation de vernis pour fils metalliques a lubrifiant interne Download PDF

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Publication number
EP0823120B1
EP0823120B1 EP96914118A EP96914118A EP0823120B1 EP 0823120 B1 EP0823120 B1 EP 0823120B1 EP 96914118 A EP96914118 A EP 96914118A EP 96914118 A EP96914118 A EP 96914118A EP 0823120 B1 EP0823120 B1 EP 0823120B1
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EP
European Patent Office
Prior art keywords
weight
wire enamel
polyethylene wax
wire
wetting agent
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.)
Expired - Lifetime
Application number
EP96914118A
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German (de)
English (en)
Other versions
EP0823120A1 (fr
Inventor
Klaus-Wilhelm Lienert
Irmgart Gebert
Helmut Lehmann
Michael W. MÜLLER
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.)
Altana Electrical Insulation GmbH
Original Assignee
Dr Beck & Co AG
Beck & Co AG Dr
Dr Beck & Co AG
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Publication of EP0823120A1 publication Critical patent/EP0823120A1/fr
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Anticipated expiration legal-status Critical
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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/308—Wires with resins

Definitions

  • the present invention relates to a wire enamel formulation containing components known per se with an internal lubricant.
  • Lacquered copper wires are coated with a lubricant around their Improve workability.
  • Classic lubricants consist of one 0.5 to 2% solution of paraffins or waxes in one easy volatile solvent. This evaporates when applied to the wire The paraffin or wax film remains solvent and back.
  • a disadvantage this method is that the usual solvents used Can cause surface cracks in the wire enamel film.
  • a lubricant which consists of a aliphatic hydrocarbon mixture as solvent and 1% Paraffin wax and 1% hydrogenated triglyceride.
  • the Paraffin wax has a melting point of 50-52 ° C.
  • the hydrated Triglyceride is a commercial product with a melting point of 47 ° C to 50 ° C.
  • This solution is made with a polyamideimide coated wire applied.
  • an internal Lubricants are used. This is in a concentration of 1% added to the polyamideimide.
  • the internal lubricant consists of Tall oil fatty acid esters. Information on the friction coefficients achieved are not made.
  • EP 00 72 178A describes the modification of wire enamel binders described in which in the polymer a C21 hydrocarbon chain is installed. This chain leads to one in the enamelled wires improved coefficient of friction. There is no information in the script to the thermal properties. It can be assumed that the Softening of the paint film and the dielectric loss factor due to the Introduction of the hydrocarbon chain suffer.
  • EP 0 103 307A describes conventionally applied lubricants described that on the wires in relays to a reduced Outgassing tend. This is achieved through the substitution of the terminal hydrogen in a polypropylene glycol through a organic rest.
  • JP 0 524 7374A Another document (JP 0 524 7374A) describes how the Use of dispersions of fluorinated waxes in conventional wire enamels the lubricity of the manufactured with it Wires is improved. However, such systems tend to separate of phases.
  • JP 0 521 7427A describes the use of a polyethylene wax dispersion described in a polyamideimid wire enamel. Experience shows, that these systems are not stable in storage.
  • an optimal Lubricant must be an internal lubricant.
  • the addition, which improves lubricity be a polymeric material and which Formulation should be stable on storage.
  • the object of the present invention was accordingly a Wire enamel formulation containing components known per se and a to provide internal lubricant to those mentioned Requirements fulfilled.
  • the internal lubricant a polyethylene wax, preferably with a Molecular mass [Mw] from 3000 to 6000 [g / mol], and as a wetting agent, a fatty alcohol ethoxylate.
  • the lubricant can also be obtained exclusively from Polyethylene wax and the wetting agent exist.
  • wire enamels with a polyesterimide as a binder be used.
  • polyesterimide resins are known and described for example in DE-OS 14 45 263 and DE-OS 14 95 100.
  • the polyesterimides are prepared in a known manner by esterifying the polyhydric carboxylic acids with the polyhydric alcohols, if appropriate with the addition of oxycarboxylic acids, and using starting materials containing imide groups. Instead of the free acids and / or alcohols, their reactive derivatives can also be used.
  • Terephthalic acid is preferably used as the carboxylic acid component, and ethylene glycol, glycerol and tris (2-hydroxyethyl) isocyanurate (THEIC) are preferably used as polyhydric alcohols, the latter being particularly preferred.
  • TEEIC 2,2-hydroxyethyl) isocyanurate
  • the use of tris (2-hydroxyethyl) isocyanurate leads to an increase in the softening temperature of the paint film obtained.
  • the starting materials containing imide groups can be, for example, by Reaction between compounds are obtained, one of which a five-membered, cyclic carboxylic acid anhydride grouping and must have at least one other functional group, while the other, apart from a primary amino group, at least one contains another functional group.
  • These other functional groups are mainly carboxyl groups or hydroxyl groups, but can also other primary amino groups or carboxylic anhydride groups his.
  • Examples of compounds with a cyclic Carboxylic anhydride grouping with a further functional group are, above all, pyromellitic dianhydride and trimellitic anhydride.
  • aromatic carboxylic anhydrides also come in Question, for example the naphthalene tetracarboxylic acid dianhydrides or Dianhydrides of tetracarboxylic acids with two benzene nuclei in the molecule, in which the carboxyl groups are in the 3,3'-, 4- and 4'-positions.
  • Examples of compounds with a primary amino group and one further functional groups are in particular diprimary diamines, for example Ethylene diamine, tetramethylene diamine, hexamethylene diamine, Nonamethylene diamine and other aliphatic diprimary diamines.
  • diprimary diamines for example Ethylene diamine, tetramethylene diamine, hexamethylene diamine, Nonamethylene diamine and other aliphatic diprimary diamines.
  • aromatic diprimary diamines such as benzidine, Diaminodiphenylmethane, diaminodiphenyl ketone, sulfone, sulfoxide, ether and thioethers, phenylenediamines, toluenediamines, xylylenediamines and also diamines with three benzene nuclei in the molecule, such as bis- (4-aminophenyl) - ⁇ , ⁇ '-p-xylene or bis (4-aminophenoxy) -1,4-benzene, and finally cycloaliphatic diamines, such as 4,4'-dicyclohexylmethane diamine.
  • amino group-containing compounds with another functional Group also amino alcohols can be used, for.
  • transesterification catalysts are used to produce the polyesterimide resins used, for example heavy metal salts, such as Lead acetate, zinc acetate, also organic titanates, cerium compounds and organic acids, such as. B. para-toluenesulfonic acid.
  • heavy metal salts such as Lead acetate, zinc acetate
  • organic titanates such as cerium compounds
  • organic acids such as. B. para-toluenesulfonic acid.
  • Crosslinking catalysts in the curing of the polyesterimides can the same transesterification catalysts - conveniently in one Proportion up to 3% by weight, based on the binder, can be used.
  • Solvents suitable for the production of polyesterimide wire enamels are cresolic and non-cresolic organic solvents like for example cresol, phenol, glycol ethers such as. B. methyl glycol, Ethyl glycol, isopropyl glycol, butyl glycol, methyl diglycol, ethyl diglycol, Butyl diglycol; Glycol ether esters, e.g. Methyl glycol acetate, Ethyl glycol acetate, butyl glycol acetate and 3-methoxy-n-butyl acetate; cyclic carbonates, such as B. propylene carbonate; cyclic esters such as B.
  • Aromatic solvents if appropriate in combination with the solvents mentioned, Examples of such solvents are xylene, Solventnaphtha®, toluene, Ethylbenzene, cumene, heavy benzene, various Solvesso® and Shellsol® types and Deasol®.
  • wire enamels with a polyamideimide can also be used as Binders can be used.
  • Such used in wire enamels Polyamideimides are known and for example in US-A-3,554,984, DE-A-24 41 020, DE-A-25 56 523, DE-A-12 66 427 and DE-A-19 56 512 described.
  • the polyamideimides are prepared in a known manner Polycarboxylic acids or their anhydrides, in which 2 carboxyl groups standing in the vicinal position and at least one more must have functional group and polyamines with at least a primary amino group capable of imide ring formation or from Compounds with at least 2 isocyanate groups.
  • the polyamide imides can also by reacting polyamides, polyisocyanates, the contain at least 2 NCO groups, and cyclic Dicarboxylic acid anhydrides which contain at least one further condensation or contain an addable group.
  • polyamideimides from diisocyanates or Manufacture diamines and dicarboxylic acids if any of the components already contains the imide group. So in particular, first one Tricarboxylic anhydride with a diprimeric diamine to the corresponding diimidocarboxylic acid are then implemented with a diisocyanate to the polyamideimide.
  • Tricarboxylic acids are preferred for the production of the polyamideimides or their anhydrides used, in which 2 carboxyl groups in vicinal Position.
  • the corresponding aromatic ones are preferred Tricarboxylic anhydrides such as e.g. Trimellitic anhydride, Naphthalene tricarboxylic acid anhydrides, bisphenyl tricarboxylic acid anhydrides as well as other tricarboxylic acids with 2 benzene nuclei in the molecule and 2 vicinal carboxyl groups, such as those listed in DE-OS 19 56 512 Examples. Trimellitic anhydride is very particularly preferred used.
  • the amine component used in the polyamidocarboxylic acids Diprimary diamines already described used become.
  • Aromatic diamines can also be used containing a thiadiazole ring, e.g. 2,5-bis (4-aminophenyl) -1,3,4-thiadiazole, 2,5-bis (3-aminophenyl) -3,3,4-thiadiazole, 2- (4-aminophenyl) -5- (3-aminophenyl) -1,3,4-thiadiazole and mixtures of the different isomers.
  • a thiadiazole ring e.g. 2,5-bis (4-aminophenyl) -1,3,4-thiadiazole, 2,5-bis (3-aminophenyl) -3,3,4-thiadiazole, 2- (4-aminophenyl) -5- (3-aminophenyl) -1,3,4-thiadiazole and mixtures of the different isomers.
  • Suitable diisocyanates for the preparation of the polyamideimides are aliphatic diisocyanates, e.g. Tetramethylene, hexamethylene, Heptamethylene and trimethylhexamethylene diisocyanates; cycloaliphatic diisocyanates, e.g. Isophorone diisocyanate, ⁇ , ⁇ '-diisocyanate-1,4-dimethylcyclohexane, Cyclohexane-1,3-, cyclohexane-1,4-, 1-methylcyclohexane-2,4- and dicyclohexylmethane-4,4'-diisocyanate; aromatic diisocyanates, e.g.
  • Phenylene, toluene, naphthylene and xylylene diisocyanates and substituted aromatic systems such as e.g. Diphenyl ether, diphenyl sulfide, diphenyl sulfone and Diphenylmethane diisocyanates; mixed aromatic-aliphatic and aromatic-hydroaromatic diisocyanates, e.g. 4-phenyl isocyanate methyl isocyanate, Tetrahydronaphthylene-1,5-, Hexahydrobenzidine 4,4'-diisocyanate. 4,4'-diphenylmethane diisocyanate, 2,4- and 2,6-tolylene diisocyanate and Hexamethylene diisocyanate used.
  • Diphenyl ether, diphenyl sulfide, diphenyl sulfone and Diphenylmethane diisocyanates mixed aromatic-aliphatic and aromatic-hydroaromatic diiso
  • Suitable polyamides are those polyamides that pass through Polycondensation of dicarboxylic acids or their derivatives with Diamines or of aminocarboxylic acids and their derivatives, such as Lactams.
  • crosslinking catalysts in the curing of the polyamide imides heavy metal salts soluble in the wire enamels, e.g. Zinc octoate, cadmium octoate, tetraisopropyl titanate or tetrabutyl titanate in an amount of up to 3% by weight, based on the binder, be used.
  • heavy metal salts soluble in the wire enamels e.g. Zinc octoate, cadmium octoate, tetraisopropyl titanate or tetrabutyl titanate in an amount of up to 3% by weight, based on the binder, be used.
  • the internal lubricant is preferably 0.1 up to 4.5% by weight of polyethylene wax and 0.1 to 2.0% by weight of wetting agent. 1.0 to 2.2% by weight of polyethylene wax are very particularly preferred and 0.2 to 1.2 wt% wetting agent.
  • the quantities indicated are each based on the proportion of binder in the wire enamel.
  • polyethylene waxes which can be used according to the invention are commercially available available under the name Luwax®. These polyethylene waxes are characterized by a narrow molar mass distribution. Furthermore high hardness and high crystallinity can be specifically set.
  • phase separation takes place.
  • a wetting agent added the phase separation can be different suppress.
  • the wire enamel formulation is accordingly in accordance with the invention Wetting agent added.
  • Wetting agent added.
  • Advantageously come in particular for this Fatty alcohol ethoxylates are used.
  • Emulan® AF a product of BASF AG, is particularly well suited to the polyethylene waxes described to stabilize a wire enamel.
  • wetting agents also include the BASF products Emulan® EL, Emulan® PO and Pluronic® 8100.
  • the present invention further relates to a method for producing the wire enamel formulation described.
  • a first Polyethylene wax preferably with a molecular mass of 3000 to 6000 [g / mol] mixed with solvent.
  • solvent Preferably 5 to 25 %
  • solvent based on the polyethylene wax, was added.
  • a proportion of solvent of 8 to 11% by weight is particularly preferred.
  • 10% by weight is very particularly preferred.
  • Prefers are mainly xylene and toluene.
  • polyethylene wax and solvents heated, preferably to 70 to 100 ° C. Is very particularly preferred a temperature of approx. 80 ° C. After the polyethylene wax is completely dissolved, is cooled back to room temperature.
  • a fatty alcohol ethoxylate is then added as a wetting agent.
  • the proportions are chosen so that preferably 0.1 to 4.5% by weight of polyethylene wax and 0.1 to 2.0% by weight of wetting agent, based in each case on the binder content in the wire enamel, are used. 1.0 to 2.2% by weight of polyethylene wax and 0.2 to 1.2% by weight of wetting agent are very particularly preferred.
  • Wire enamels are considered, which are described as binders above Contain polyester imides or polyester amide imides.
  • wire enamels according to the invention thus produced are found in particular Use in the coating of electrical conductors.
  • Example 1 Production of a polyesterimide wire enamel
  • polyesterimide is made up of 56 parts of a mixture Kresol / Solventnaphtha® dissolved in a ratio of 2: 1 and with 0.7% on the Overall recipe, a commercially available titanium catalyst.
  • the way The wire enamel obtained has a viscosity of 800 mPas (23 ° C) Solids content of 39% (1g / 1h / 180 ° C).
  • a polyamideimide is described in DE-AS 12 66 427 Method from 38.5 parts of trimellitic acid and 60.0 parts of diphenylmethane diisocyanate manufactured.
  • the wire enamel is a 25% solution this polyamideimide in a mixture of 65 parts of N-methylpyrrolidone and 35 parts of xylene. This wire enamel has a viscosity of 23 ° C 230 mPas on.
  • Example 5 Production of a polyesterimide wire enamel with internal lubricant
  • Example 6 Production of a polyamideimide wire enamel with internal lubricant
  • a piece of wire of approx. 750 mm length becomes, as in IEC 851-5 / 4.3 described a twist made.
  • the twist becomes 240 mm cut out. This section has 10 turns.
  • the opposite ends of the wires from the twist are in one Tearing machine Lloyd M30K clamped. It becomes the force in Newtons measured around the twist at a speed of 200 m / min pull apart.
  • the average force for a standard wire was 2.5 Newtons measured.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Insulated Conductors (AREA)
  • Paints Or Removers (AREA)
  • Lubricants (AREA)
  • Organic Insulating Materials (AREA)
  • Metal Extraction Processes (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Claims (10)

  1. Formulation de laque pour fils contenant des composants connus en soi et au moins un lubrifiant interne, caractérisée en ce que le lubrifiant contient une cire de polyéthylène, présentant de préférence une masse moléculaire de 3000 à 6000 [g/mole] et comme mouillant un éthoxylate d'alcool gras.
  2. Formulation de laque pour fils selon la revendication 1, caractérisée en ce que le lubrifiant est constitué de 0,1 à 4,5% en poids, de préférence de 1,0 à 2,2% en poids, de cire de polyéthylène et de 0,1 à 2,0% en poids, de préférence de 0,2 à 1,2% en poids, de mouillant, les % en poids étant à chaque fois rapportés à la proportion de liant dans la laque pour fils.
  3. Formulation de laque pour fils selon l'une quelconque des revendications 1 ou 2, caractérisée en ce qu'elle contient un polyesterimide ou un polyamideimide comme liant.
  4. Procédé pour la préparation d'une formulation de laque pour fils selon l'une quelconque des revendications 1 à 3, caractérisé
    a) en ce qu'on mélange, à une cire de polyéthylène, présentant de préférence une masse moléculaire de 3000 à 6000 [g/mole], un solvant, de préférence en une quantité de 5 à 25% en poids par rapport à la cire de polyéthylène,
    b) en ce qu'on chauffe le tout, de préférence à 70 jusqu'à 100°C,
    c) en ce qu'on refroidit le tout après la dissolution complète de la cire de polyéthylène,
    d) en ce qu'on ajoute de l'éthoxylate d'alcool gras comme mouillant et
    e) en ce qu'on ajoute la dispersion ainsi obtenue à la laque pour fils contenant des composants connus en soi.
  5. Procédé selon la revendication 4, caractérisé en ce que la proportion du solvant ajoutée à la cire de polyéthylène est de 8 à 11% en poids, de préférence de 10% en poids.
  6. Procédé selon l'une quelconque des revendications 4 ou 5, caractérisé en ce qu'on utilise du xylène ou du toluène comme solvant.
  7. Procédé selon l'une quelconque des revendications 4 à 6, caractérisé en ce qu'on chauffe jusqu'environ 80°C dans l'étape b).
  8. Procédé selon l'une quelconque des revendications 4 à 7, caractérisé en ce qu'on utilise un lubrifiant constitué de 0,1 à 4,5% en poids, de préférence de 1,0 à 2,2% en poids, de cire de polyéthylène et de 0,1 à 2,0% en poids, de préférence de 0,1 à 1,2% en poids, de mouillant, les % en poids étant à chaque fois rapportés à la proportion de liant dans la laque pour fils.
  9. Procédé selon l'une quelconque des revendications 4 à 8, caractérisé en ce qu'on utilise une laque pour fils contenant comme liant un polyesterimide ou un polyamideimide.
  10. Utilisation de la laque pour fils selon les revendications 6 ou 7 pour le revêtement de conducteurs électriques.
EP96914118A 1995-04-26 1996-04-25 Formulation de vernis pour fils metalliques a lubrifiant interne Expired - Lifetime EP0823120B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19515263A DE19515263A1 (de) 1995-04-26 1995-04-26 Drahtlackformulierung mit internem Gleitmittel
PCT/EP1996/001723 WO1996034399A1 (fr) 1995-04-26 1996-04-25 Formulation de vernis pour fils metalliques a lubrifiant interne
DE19515263 1998-04-04

Publications (2)

Publication Number Publication Date
EP0823120A1 EP0823120A1 (fr) 1998-02-11
EP0823120B1 true EP0823120B1 (fr) 2001-08-08

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP96914118A Expired - Lifetime EP0823120B1 (fr) 1995-04-26 1996-04-25 Formulation de vernis pour fils metalliques a lubrifiant interne

Country Status (10)

Country Link
US (1) US6022918A (fr)
EP (1) EP0823120B1 (fr)
JP (1) JPH11504156A (fr)
KR (1) KR100382621B1 (fr)
AT (1) ATE204093T1 (fr)
BR (1) BR9608294A (fr)
DE (2) DE19515263A1 (fr)
ES (1) ES2163626T3 (fr)
TW (1) TW315387B (fr)
WO (1) WO1996034399A1 (fr)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19648830A1 (de) * 1996-11-26 1998-05-28 Beck & Co Ag Dr Verfahren zur Herstellung carboxyl- und hydroxylgruppenhaltiger Polyesterimide und deren Verwendung in Drahtlacken
US6392000B1 (en) 2000-10-26 2002-05-21 E. I. Du Pont De Nemours And Company Binder for a coating composition for electrical conductors
US7099627B2 (en) * 2003-06-11 2006-08-29 Acco Brands Usa Llc Systems and methods for a wireless network connection point locator
US7396395B1 (en) * 2007-05-08 2008-07-08 Everest Textile Co., Ltd. Composition of a water-repellent agent
DE102010039169A1 (de) 2010-08-10 2012-02-16 Universität Paderborn Selbststrukturierende Oberflächen durch PDMS-Phasentrennungen in harten Polymerbeschichtungen
DE102010039168A1 (de) 2010-08-10 2012-02-16 Schwering & Hasse Elektrodraht Gmbh Elektroisolierlacke aus modifizierten Polymeren und daraus hergestellte elektrische Leiter mit verbesserter Gleitfähigkeit
US10406791B2 (en) 2011-05-12 2019-09-10 Elantas Pdg, Inc. Composite insulating film
US10253211B2 (en) 2011-05-12 2019-04-09 Elantas Pdg, Inc. Composite insulating film
EP4307322A1 (fr) * 2022-07-13 2024-01-17 Siemens Aktiengesellschaft Fil rond isolé par un vernis, procédé de fabrication et utilisation correspondante

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US4450258A (en) * 1975-01-02 1984-05-22 General Electric Company Coating compositions
US4146499A (en) * 1976-09-18 1979-03-27 Rosano Henri L Method for preparing microemulsions
JPS5826409A (ja) * 1981-08-07 1983-02-16 住友電気工業株式会社 絶縁電線
US4390590A (en) * 1981-10-19 1983-06-28 Essex Group, Inc. Power insertable polyamide-imide coated magnet wire
CA1200587A (fr) * 1982-09-14 1986-02-11 Tatsumi Ide Fil de bobine pour dispositif electrique scelle
DE3635141C1 (de) * 1986-10-15 1988-03-03 Pelikan Ag Thermocarbonband mit einer kunststoffgebundenen Aufschmelzfarbe sowie ein Verfahren zur Herstellung dieses Bandes
DE3765390D1 (de) * 1986-11-11 1990-11-08 Sumitomo Electric Industries Wickeldraht und diesen verwendendes elektromagnetisches relais.
JPH05217427A (ja) * 1992-02-04 1993-08-27 Furukawa Electric Co Ltd:The 自己潤滑性絶縁電線
JPH05247374A (ja) * 1992-03-03 1993-09-24 Fujikura Ltd 潤滑塗料およびこれを用いた自己潤滑絶縁電線
DE4330342A1 (de) * 1993-09-08 1995-03-09 Basf Ag Stabile wäßrige Polyolefinwachsdispersionen

Also Published As

Publication number Publication date
DE59607451D1 (de) 2001-09-13
US6022918A (en) 2000-02-08
EP0823120A1 (fr) 1998-02-11
TW315387B (fr) 1997-09-11
ES2163626T3 (es) 2002-02-01
KR100382621B1 (ko) 2005-05-24
WO1996034399A1 (fr) 1996-10-31
JPH11504156A (ja) 1999-04-06
BR9608294A (pt) 1999-05-11
ATE204093T1 (de) 2001-08-15
KR19990008063A (ko) 1999-01-25
DE19515263A1 (de) 1996-10-31

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