EP0301120B1 - Lubrifiant pour le formage à froid de matériaux métalliques et son procédé de fabrication - Google Patents

Lubrifiant pour le formage à froid de matériaux métalliques et son procédé de fabrication Download PDF

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Publication number
EP0301120B1
EP0301120B1 EP87110995A EP87110995A EP0301120B1 EP 0301120 B1 EP0301120 B1 EP 0301120B1 EP 87110995 A EP87110995 A EP 87110995A EP 87110995 A EP87110995 A EP 87110995A EP 0301120 B1 EP0301120 B1 EP 0301120B1
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Prior art keywords
water
polyvinyl alcohol
lubricant
groups
weight
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Expired - Lifetime
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EP87110995A
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German (de)
English (en)
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EP0301120A1 (fr
Inventor
Heinz-Rüdiger Dr.rer.nat. Vogel
Jürgen Dipl.-Chem. Reichert
Klaus Dipl.-Chem. Schipschack
Harri Dr.-Ing. Weinhold
Dieter Rauschenbach
Harald Dr.Rer.Nat. Genest
Bernhard Dipl.-Phys. Kurze
Jörg Dr.-Ing. Eickemeyer
Ingeborg Sasse
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Ecoform Umformtechnik GmbH
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Ecoform Umformtechnik GmbH
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Priority to EP87110995A priority Critical patent/EP0301120B1/fr
Priority to AT87110995T priority patent/ATE81528T1/de
Priority to DE8787110995T priority patent/DE3782252D1/de
Publication of EP0301120A1 publication Critical patent/EP0301120A1/fr
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00Lubricating compositions containing more than 10% water
    • C10M173/02Lubricating compositions containing more than 10% water not containing mineral or fatty oils
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26Compounds containing silicon or boron, e.g. silica, sand
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    • C10M129/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26Carboxylic acids; Salts thereof
    • C10M129/28Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/38Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
    • C10M129/40Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms monocarboxylic
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    • C10M129/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26Carboxylic acids; Salts thereof
    • C10M129/56Acids of unknown or incompletely defined constitution
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    • C10M145/00Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
    • C10M145/02Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/04Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an alcohol, aldehyde, ketonic, ether, ketal or acetal radical
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02Water
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
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    • C10M2201/087Boron oxides, acids or salts
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    • C10M2201/10Compounds containing silicon
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    • C10M2201/102Silicates
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    • C10M2201/105Silica
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/04Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an alcohol or ester thereof; bound to an aldehyde, ketonic, ether, ketal or acetal radical
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/06Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/06Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
    • C10M2209/062Vinyl esters of saturated carboxylic or carbonic acids, e.g. vinyl acetate
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10N2010/00Metal present as such or in compounds
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    • C10N2010/02Groups 1 or 11
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    • C10N2010/04Groups 2 or 12
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    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/24Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
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    • C10N2040/241Manufacturing joint-less pipes
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    • C10N2040/242Hot working
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    • C10N2040/243Cold working
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    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/01Emulsions, colloids, or micelles

Definitions

  • the invention relates to a liquid lubricant for the cold forming of metallic materials and its production, which is used, for example, in cold rolling, cold upsetting, thread rolling, drawing sheet metal parts, calibrating sintered bodies, stranding and bending, and in particular when drawing strand-like shaped material such as wire, profiles and Pipes, is advantageously applicable.
  • a lubricant When pulling wires, profiles, pipes, etc. a lubricant must be applied to the drawing material before the drawing tool, which is to prevent direct contact between the working surfaces of the drawing tool and the surface of the drawing material.
  • the use of solid, semi-solid or liquid lubricants at room temperature is common.
  • the liquid lubricants used include Oils, chlorinated paraffins, soap solutions and reactive fatty acid soaps are used in conjunction with a basic chemical coating.
  • Liquid lubricants are also known which consist of solid lubricants dispersed in water. In one of these lubricants, alkaline earth metal soaps are used as solid lubricants.
  • the lubricant also contains 2% by mass of polyvinyl alcohol as a dispersant for the solid lubricant, a corrosion inhibitor and surface-active substances. The lubricant is applied to the material to be formed, for example in the immersion process, and then dried, a solid lubricant film being produced for the subsequent forming process.
  • a disadvantage of this lubricant is that the dried solid lubricant film experiences a significant reduction in quality due to the thermal degradation of the polyvinyl alcohol that occurs during the shaping process, in particular with regard to its dynamic viscosity, its temperature resistance and its adhesiveness. Due to this reduction in quality, large cross-sectional reductions per train or only small total cross-sectional decreases per lubricant application are possible. In addition, this lubricant allows only low drawing speeds due to thermal degradation, and the forming of difficult-to-form materials is also critical.
  • these lubricants may also contain inorganic water-soluble salts, such as fatty acid salts, alkali phosphates, alkali borates and ammonium salts.
  • inorganic water-soluble salts such as fatty acid salts, alkali phosphates, alkali borates and ammonium salts.
  • the lignin compounds contained serve as dispersants and solubilizers for the present metal soaps.
  • the modified polyvinyl alcohols are, for example, phosphatically esterified or carboxy-modified polyvinyl alcohols, for example the ammonium salts of corresponding phosphate esters or corresponding carboxylates.
  • the alkaline earth metal soap is used as an aqueous dispersion which is prepared by dispersing the soap in water using at least one anion-active compound and / or nonionic surface-active compound.
  • the invention is based on the object of specifying a liquid lubricant which gives high-performance liquid or solid lubricating coatings on metal material to be formed, and a method for its production.
  • the object is achieved according to claims 1 and 7.
  • the dependent claims relate to advantageous embodiments.
  • both types of polyvinyl alcohols E and F preferably have a degree of polymerization in the range from 100 to 1500, the total content of polyvinyl alcohols E and F being ⁇ 3% by mass if both types are present.
  • water-insoluble fatty acid salts A are preferred Alkaline earth metal soaps and preferably technical calcium stearate are present in an amount of 3 to 8% by mass.
  • the water-soluble alkali metal soaps B advantageously contain sodium soaps, preferably technical sodium stearate.
  • Suitable glass-forming borate C are e.g. Alkali borates and preferably borax.
  • Suitable surfactants D are in particular anionic and nonionic surfactants and in particular polyethylene oxide adducts, preferably nonylphenol-polyethylene oxide adducts.
  • hydrogen peroxide oxygen, ozone, peroxides, peroxo salts, hypochlorites, chlorates, dichromates and / or permanganate
  • the preferred oxidizing agent is hydrogen peroxide.
  • the oxidizing agent is reacted with an acidic polyvinyl alcohol solution, preferably with a pH of 1.5 to 4.
  • the oxidizing agent can also be reacted with an alkaline polyvinyl alcohol solution, preferably with a pH of 8 to 12.5.
  • the oxidizing agent is first reacted with an acidic polyvinyl alcohol solution, whereupon the pH is shifted to the alkaline range during the reaction by adding alkali metal hydroxides, preferably sodium hydroxide.
  • the lubricant according to the invention has a low to high viscosity and guarantees a high coating mass and a homogeneous and thermally stable lubricant layer on the material to be formed. This enables high individual degrees of forming and forming speeds to be achieved, and the forming of difficult-to-form materials is also possible. In addition, intermediate coatings between individual forming stages can be largely avoided. If the lubricant contains structure-modified polyvinyl alcohol, there is no or only a slight tendency to form skin or gel, which has a particularly favorable effect on the coating and drying effort.
  • aqueous polyvinyl alcohol solution which contains a polyvinyl alcohol which is 2% esterified with acetate groups and which has a pH of 2.2 and a temperature of 93 ° C.
  • Hydrogen peroxide added as an oxidizing agent.
  • the solution is made alkaline with sodium hydroxide, the oxidation reaction is continued for a further 10 minutes while maintaining the specified temperature, and then an aqueous calcium soap dispersion which contains an alkylphenol-polyethylene oxide adduct as a dispersant is mixed in to prepare a lubricant concentrate.
  • This concentrate is diluted with water before use for cold forming and sodium stearate is added at a temperature of 80 ° C.
  • the ready-to-use lubricant is made from the following composition: (Dimensions-%) Structure modified polyvinyl alcohol 1.8 Calcium soap 6 Alkylphenol polyethylene oxide adduct 0.3 Sodium stearate 1 borax 5 water Rest.
  • This lubricant is used to coat 6.5 mm thick Mn 6 wire rod in a coil immersion process at 80 ° C. After drying the lubricant, which takes place in a very short time due to the inherent heat of the wire, the wire is removed in 7 steps with a pulling speed of 10 m / s on the 7th block without intermediate coating drawn to a final diameter of 2.0 mm.
  • This lubricant is used to coat 8.0 mm thick wire rod of 20 Mn B 4 Q quality in a coil immersion process at 75 ° C. After the lubricant has dried, which occurs quickly due to the inherent heat of the wire, the wire is pulled to 7.05 mm in one go. After drawing, the wire has a residual lubricant film that is sufficiently thick for further processing, for example by cold upsetting.
  • the finished lubricant is made from the following composition: (Dimensions-%) Structure modified polyvinyl alcohol 1.4 Calcium soap 6 Alkylphenol polyethylene oxide adduct 0.3 Sodium metaborate 4th Manganese dioxide hydrate 0.02 water Rest.
  • This lubricant is used to coat 5.5 mm thick wire rod of quality 10 Mn Si 6 in a coil immersion process at 85 ° C and to dry it in air. Then the coated wire is drawn in 5 steps without intermediate coating to a final diameter of 2.5 mm.
  • a lubricant is made from the following composition: (Dimensions-%) Calcium stearate 5 Sodium tetraborate decahydrate 5 Polyvinyl alcohol 1.5 water Rest.
  • the polyvinyl alcohol used is esterified to 12% with acetate groups.
  • This lubricant is used to coat 6.5 mm thick wire rod of quality C15 in a continuous process.
  • the lubricant layer is then dried and then the wire is drawn to 3.6 mm in 6 steps at a pulling speed of 7 m / s.
  • a lubricant is made from the following composition: (Dimensions-%) Calcium stearate 4th Sodium metaborate 6 Polyvinyl alcohol 1 water Rest.
  • the lubricant film is dried and the wire is pulled at a pulling speed of 6 m / s in one go to 2.0 mm in diameter.
  • a lubricant is made from the following composition: (Dimensions-%) Calcium stearate 4th Sodium metaborate 2.5 Polyvinyl alcohol 1 water Rest.
  • the polyvinyl alcohol used is 2% esterified with acetate groups.
  • a steel wire of quality C 15 Q with an initial diameter of 3.35 mm is drawn to 3.0 mm in one single step in a wet pass.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)

Claims (10)

  1. Lubrifiant pour la déformation à froid de matériaux métalliques, contenant
    (A) des sels d'acides gras insolubles dans l'eau,
    (B) 0 à 1,5 % en masse de savons de métaux alcalins solubles dans l'eau,
    (C) des borates vitrifiants
    et
    (D) 0 à 1 % en masse d'un ou plusieurs agents tensioactifs,
    caractérisés en ce qu'ils contiennent
    (E) 0,2 à 1,8 % en masse d'un ou plusieurs alcools polyvinyliques
    et/ou
    (F) 0,2 à 3 % en masse d'un alcool polyvinylique à structure modifiée par un oxydant et qui contient, outre les groupes hydroxyle déterminant la structure, des groupes céto, des groupes carboxyle et/ou des groupes d'ions carboxylate, ainsi qu'éventuellement des groupes aldéhyde et/ou des groupes oléfine conjugués avec des groupes céto,
    et
    (G) 1 à 6 % en masse d'ester borique d'alcool polyvinylique E et/ou F,
    - 1 à 45 % en masse des sels d'acides gras insolubles dans l'eau A dont 65% ou plus présentent une longueur de chaîne de 16 atomes de carbone ou plus,
    et
    - 1 à 6 % en masse de borates vitrifiants C.
  2. Lubrifiant selon la revendication 1, caractérisé en ce que les alcools polyvinyliques E et/ou F présentent un degré de polymérisation de 100 à 1500.
  3. Lubrifiant selon la revendication 1 ou 2, caractérisé en ce que lorsque les deux alcools polyvinyliques E et F sont présents, leur quantité totale est inférieure ou égale à 3 % en masse.
  4. Lubrifiant selon l'une des revendications 1 à 3, caractérisé en ce qu'il contient
    3 à 8 % en masse d'un ou plusieurs savons de métaux alcalino-terreux comme sels d'acides gras insolubles dans l'eau A, de préférence du stéarate de calcium,
    et
    un ou plusieurs savons de sels de sodium comme savons de métaux alcalins solubles dans l'eau B, de préférence du stéarate de sodium.
  5. Lubrifiant selon l'une des revendications 1 à 4, caractérisé en ce qu'il contient un borate de métal alcalin comme borate vitrifiant C, de préférence du Borax.
  6. Lubrifiant selon l'une des revendications 1 à 5, caractérisé en ce qu'il contient des agents tensioactifs anioniques ou non-ioniques, en particulier des produits d'addition d'oxyde de polyéthylène et de préférence un produit d'addition de nonylphénol-(oxyde de polyéthylène) comme agent tensioactif D.
  7. Procédé pour la fabrication du lubrifiant selon l'une des revendications 1 à 6,
    caractérisé en ce que
    (I) l'on fabrique un concentré d'alcool polyvinylique et d'eau et on modifie, au moins partiellement, la structure de l'alcool polyvinylique avec un oxydant,
    (II) l'on introduit sous agitation le concentré de l'étape I ainsi que les sels d'acides gras A et B et éventuellement les agents tensiocactifs D dans de l'eau,
    et que
    (III) l'on ajoute les borates vitrifiants C ou l'ester borique G.
  8. Procédé selon la revendication 7, caractérisé en ce qu'on emploie du peroxyde d'hydrogène, de l'oxygène, de l'ozone, des peroxydes, des peroxosels, un hypochlorite, un chlorate, un dichromate et/ou un permanganate comme oxydant dans l'étape I.
  9. Procédé selon la revendication 7 ou 8, caractérisé en ce qu'on fait réagir l'oxydant pour l'étape I avec une solution d'alcool polyvinylique rendue acide, de préférence d'un pH de 1,5 à 4, ou avec une solution d'alcool polyvinylique rendue basique, de préférence d'un pH de 8 à 12,5.
  10. Procédé selon l'une des revendications 7 à 9, caractérisé en ce qu'on fait réagir l'oxydant pour l'étape I avec une solution d'alcool polyvinylique rendue acide et qu'on abaisse le pH dans la zone alcaline durant la réaction en ajoutant des hydroxydes alcalins, de préférence de l'hydroxyde de sodium.
EP87110995A 1987-07-29 1987-07-29 Lubrifiant pour le formage à froid de matériaux métalliques et son procédé de fabrication Expired - Lifetime EP0301120B1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP87110995A EP0301120B1 (fr) 1987-07-29 1987-07-29 Lubrifiant pour le formage à froid de matériaux métalliques et son procédé de fabrication
AT87110995T ATE81528T1 (de) 1987-07-29 1987-07-29 Schmiermittel fuer die kaltumformung metallischer werkstoffe und verfahren zu seiner herstellung.
DE8787110995T DE3782252D1 (de) 1987-07-29 1987-07-29 Schmiermittel fuer die kaltumformung metallischer werkstoffe und verfahren zu seiner herstellung.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP87110995A EP0301120B1 (fr) 1987-07-29 1987-07-29 Lubrifiant pour le formage à froid de matériaux métalliques et son procédé de fabrication

Publications (2)

Publication Number Publication Date
EP0301120A1 EP0301120A1 (fr) 1989-02-01
EP0301120B1 true EP0301120B1 (fr) 1992-10-14

Family

ID=8197166

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87110995A Expired - Lifetime EP0301120B1 (fr) 1987-07-29 1987-07-29 Lubrifiant pour le formage à froid de matériaux métalliques et son procédé de fabrication

Country Status (3)

Country Link
EP (1) EP0301120B1 (fr)
AT (1) ATE81528T1 (fr)
DE (1) DE3782252D1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19508247C1 (de) * 1995-03-08 1996-11-14 Nordpol Seifenfabrik Inh Ria T Kühlschmierstoff zur Metallverformung
ATE415504T1 (de) 2005-12-22 2008-12-15 Arcelormittal France Behandlungsverfahren der metallischen oberflächen durch carboxilierung, benutzung dieses verfahrens für den zeitweiligen korrosionsschutz und verfahren zur herstellung eines geformten carboxylierten bleches
CN107446660A (zh) * 2017-07-24 2017-12-08 浙江宝晟铁路新材料科技有限公司 一种聚乙烯醇缩醛基固体润滑剂及其制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3052662A (en) * 1959-06-30 1962-09-04 Kurashiki Rayon Co Polyvinyl alcohol product and process for making the same
FR1266125A (fr) * 1960-08-25 1961-07-07 Aluminum Res Corp Nouveaux lubrifiants pour la déformation à froid des métaux et procédé pour leur application
GB1059569A (en) * 1962-12-07 1967-02-22 Canning & Co Ltd W Improvements in cadmium electroplating and in polyvinyl alcohol derivatives for use therein
JPS494108B1 (fr) * 1970-08-15 1974-01-30
JPS5038672A (fr) * 1973-08-09 1975-04-10

Also Published As

Publication number Publication date
ATE81528T1 (de) 1992-10-15
DE3782252D1 (de) 1992-11-19
EP0301120A1 (fr) 1989-02-01

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