EP3124582A1 - Wässriges schmierbeschichtungsmittel mit ausgezeichneter korrosionsbeständigkeit und bearbeitbarkeit sowie metallmaterial - Google Patents

Wässriges schmierbeschichtungsmittel mit ausgezeichneter korrosionsbeständigkeit und bearbeitbarkeit sowie metallmaterial Download PDF

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Publication number
EP3124582A1
EP3124582A1 EP15768354.1A EP15768354A EP3124582A1 EP 3124582 A1 EP3124582 A1 EP 3124582A1 EP 15768354 A EP15768354 A EP 15768354A EP 3124582 A1 EP3124582 A1 EP 3124582A1
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Prior art keywords
water
lubricating coating
coating agent
based lubricating
comparative example
Prior art date
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EP15768354.1A
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English (en)
French (fr)
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EP3124582A4 (de
EP3124582B1 (de
Inventor
Tsuyoshi Hatakeyama
Shinobu Komiyama
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Nihon Parkerizing Co Ltd
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Nihon Parkerizing Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00—Lubricating compositions containing more than 10% water
    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J3/00—Lubricating during forging or pressing
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/24—Compounds containing phosphorus, arsenic or antimony
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
    • C—CHEMISTRY; METALLURGY
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    • C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
    • C10M143/02—Polyethene
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    • C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/04—Macromolecular 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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    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
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    • C10M125/02—Carbon; Graphite
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    • C10M125/22—Compounds containing sulfur, selenium or tellurium
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    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/16—Amides; Imides
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    • C10M133/38—Heterocyclic nitrogen compounds
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    • C10M133/42—Triazines
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    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/10—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate
    • C10M145/12—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate monocarboxylic
    • C10M145/14—Acrylate; Methacrylate
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    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10M145/16—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate polycarboxylic
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    • C10M145/18—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/20—Condensation polymers of aldehydes or ketones
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    • C10M145/22—Polyesters
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    • C10M159/02—Natural products
    • C10M159/06—Waxes, e.g. ozocerite, ceresine, petrolatum, slack-wax
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    • C10M2209/101—Condensation polymers of aldehydes or ketones and phenols, e.g. Also polyoxyalkylene ether derivatives thereof
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/102—Polyesters
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/221—Six-membered rings containing nitrogen and carbon only
    • C10M2215/222—Triazines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/042—Metal salts thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating

Definitions

  • the present invention relates to a water-based lubricating coating agent which is applied when plastic working is performed to various types of metal materials, and a metal material with a coating film formed by applying the agent onto the metal material surface and drying the agent.
  • chemical conversion coating films are common which are composite coating films using phosphate coating films and soaps.
  • the chemical conversion coating films have problems such as by-products associated with reactions with metal materials, effluent treatments of water such as water rinsing, and large spaces for the treatments, and in recent years, environmentally conscious water-based dry-in-place type one-pack lubricants have been developed.
  • Patent Literature 1 discloses a water-based lubricating coating agent for plastic working of metal materials, characterized in that the composition of (A) water-soluble inorganic salt and (B) a wax is dissolved or dispersed in water, and the solid content mass ratio (B)/(A) falls within the range of 0.3 to 1.5, and a method of forming a coating film therefrom.
  • Patent Literature 2 discloses a water-based lubricating coating agent for plastic working of metal materials, which contains an alkali metal borate (A), characterized in that the alkali metal borate (A) includes a lithium borate, the molar ratio of lithium to all of the alkali metals is 0.1 to 1.0 in the alkali metal borate (A), and the molar ratio (B/M) between a boric acid B and an alkali metal M is 1.5 to 4.0 in the alkali metal borate (A), and a method of forming a coating film therefrom.
  • This technique is supposed to suppress the crystallization of the coating film, which is caused by moisture absorption of the coating film, thereby making it possible to form coating films with not only workability but also high corrosion resistance.
  • Patent Literature 3 discloses a non-phosphorus aqueous lubricant for plastic working, which contains A component: inorganic solid lubricant, B component: wax, and C component: water-soluble inorganic metal salt, characterized in that the solid content mass ratio (A component/B component) is 0.1 to 5 between the A component and the B component, and the solid content mass ratio (C component/(A component + B component + C component)) of the C component is 1 to 30% to the total amount of the A component, B component, and C component.
  • This technique is directed to a lubricant containing no phosphorus, and supposed to be able to achieve corrosion resistance comparable to that of chemical conversion coating films.
  • Patent Literature 4 discloses a water-based lubricating coating agent including a water-soluble inorganic salt (A), a lubricant (B) selected from molybdenum disulfide and graphite, and a wax (C) dissolved or dispersed in water, where the ratio (B)/(A) is 1.0 to 5.0 in terms of solid content weight ratio, and the ratio (C)/(A) is 0.1 to 1.0 in solid content weight ratio, and a method of forming a coating film therefrom.
  • This technique is supposed to achieve the same level of high workability as that of chemical conversion coating films by blending a conventional water-based lubricating coating agent with molybdenum disulfide or graphite.
  • the inventors have found, as a result of earnestly studying in order to solve the problems mentioned above, that the formation of a coating film by combining a water-soluble silicate and a specific water-soluble inorganic salt at a specific ratio provides high corrosion resistance (in particular, long-term rust prevention property), workability and adequate film removability which have not been able to be achieved in any way by the single components, thereby achieving the present invention.
  • the present invention (1) is a water-based lubricating coating agent characterized in that a water-soluble silicate (A) and at least one water-soluble inorganic salt (B) selected from a tungstate, a phosphate and a borate are blended such that the solid content mass ratio (B)/(A) falls within the range of 0.7 to 25.
  • A water-soluble silicate
  • B water-soluble inorganic salt
  • the present invention (2) is the water-based lubricating coating agent according to the invention (1), which is characterized in that the agent includes a resin component (C), and the solid content mass ratio (C)/ ⁇ (A) + (B) ⁇ is 0.01 to 3.
  • the present invention (3) is the water-based lubricating coating agent according to the invention (2), characterized in that the resin component (C) is at least one selected from the group consisting of a vinyl resin, an acrylic resin, an epoxy resin, an urethane resin, a phenolic resin, a cellulose derivative, a polymaleic acid, a polyolefin, and a polyester.
  • the resin component (C) is at least one selected from the group consisting of a vinyl resin, an acrylic resin, an epoxy resin, an urethane resin, a phenolic resin, a cellulose derivative, a polymaleic acid, a polyolefin, and a polyester.
  • the present invention (4) is the water-based lubricating coating agent according to the inventions (1)-(3), characterized in that the agent includes a lubricant (D), and the solid content mass ratio (D)/ ⁇ (A) + (B) ⁇ is 0.01 to 6.
  • the present invention (5) is the water-based lubricating coating agent according to the invention (4), characterized in that the lubricant (D) is at least one selected from the group consisting of a wax, polytetrafluoroethylene, a fatty acid soap, a fatty acid metal soap, a fatty acid amide, molybdenum disulfide, tungsten disulfide, graphite, melamine cyanurate, an amino acid compound of layered structure, and a layered clay mineral.
  • the lubricant (D) is at least one selected from the group consisting of a wax, polytetrafluoroethylene, a fatty acid soap, a fatty acid metal soap, a fatty acid amide, molybdenum disulfide, tungsten disulfide, graphite, melamine cyanurate, an amino acid compound of layered structure, and a layered clay mineral.
  • the present invention (6) is a metal material with a lubricating coating film of 0.5 to 40 g/m 2 as coating weight, which is formed on a metal material surface by applying and drying the water-based lubricating coating agent for plastic working according to the inventions (1)-(5), which is excellent in plastic workability.
  • the use of the water-based lubricating coating agent according to the present invention provides a lubricating coating film which is excellent in corrosion resistance, workability and film removability in practical use.
  • the agent is significantly superior as compared with conventional water-based lubricating coating films in that all of these performances have a level comparable or superior to those of chemical conversion coating films.
  • Metal materials where the coating film with the previously mentioned great characteristics is formed on the metal material surfaces can be obtained by applying and drying the water-based lubricating coating agent according to the present invention.
  • Fig. 1 is indications of the evaluation in an upsetting-ball ironing tribo-test (seizure resistance evaluation).
  • a water-based lubricating coating agent according to the present invention is obtained by blending a water-soluble silicate (A) (hereinafter, referred to as a silicate (A)) and at least one water-soluble inorganic salt (B) (hereinafter, referred to as an inorganic salt (B)) selected from a tungstate, a phosphate and a borate such that the solid content mass ratio (B)/(A) falls within the range of 0.7 to 25.
  • the blend in the range can form a coating film with high corrosion resistance and workability and adequate film removability which have not been able to be achieved by the silicate (A) or inorganic salt (B) itself.
  • water-soluble in the Claims and the Specification means that the solubility in water at room temperature (25°C) ⁇ the mass (g) of a solute dissolved in 100 g of water ⁇ is at least 1 g, and preferably 10 g or more.
  • the inorganic salt (B) When the silicate (A) and the inorganic salt (B) are combined to provide a coating film, the inorganic salt (B) will be incorporated finely and homogeneously in a network structure formed by the silicate (A). As a result, the fragile coating film of the silicate (A) is made flexible to improve the workability.
  • the incorporation of the inorganic salt (B) in the network structure of the silicate (A) makes the coating film denser, thereby enhancing the barrier performance, and thus improving the corrosion resistance (in particular, long-term rust prevention property).
  • the network structure of the silicate (A) is appropriately blocked by the inorganic salt (B), thereby improving the film removability.
  • the ratio between the silicate (A) and the inorganic salt (B) is important for delivering the performances mentioned above.
  • the performances are delivered at a solid content mass ratio (B)/(A) within the range of 0.7 to 25, but preferably in the range of 0.9 to 10.0, and more preferably 1.1 to 3.0.
  • the ratio (B)/(A) below 0.7 results in failure to achieve sufficient corrosion resistance and workability, and also provides a coating film which is inferior in film removability. This is due to a rigid network structure formed by the relatively increased amount of the silicate.
  • the ratio (B)/(A) in excess of 25 results in failure to achieve sufficient corrosion resistance, and also results in a coating film which is inferior in adhesion and uniformity. This is due to the fact that the relatively excessively small amount of the silicate results in failure to build an adequate network structure, thereby degrading the barrier performance, and degrading the adhesion and uniformity of the coating film.
  • the corrosion resistance is significantly improved by the formation of a passivation film that has a self-repairing function unique to tungsten.
  • stable corrosion resistance can be achieved even when the coating film becomes defective, e.g., due to steels in contact with each other. For this reason, stable corrosion resistance is likely to be produced even in the case of processing large amounts of materials simultaneously, such as mass processing and coil processing of wire rods with the use of barrels for use in lubricating agents for cold forging.
  • silicate (A) for use in the coating agent according to the present invention examples include, for example, lithium silicates, sodium silicates, and potassium silicates. These may be used singly, or two or more thereof may be combined. In particular, it is preferable to use lithium silicates and/or sodium silicates.
  • Tungstates include, for example, lithium tungstates, sodium tungstates, potassium tungstates, and ammonium tungstates.
  • Phosphates include, for example, ammonium phosphates, lithium phosphates, sodium phosphates, and potassium phosphates.
  • the phosphates include salts of condensed phosphoric acids such as a tripolyphosphoric acid, a metaphosphoric acid, and a pyrophosphosric acid.
  • Borates include, for example, sodium borates (e.g., sodium tetraborate), potassium borates (e.g., potassium tetraborate), and ammonium borates (e.g., ammonium tetraborate). These may be used singly, or two or more thereof may be combined.
  • the resin component (C) is blended for purpose of providing binder action, improving the adhesion between the base material and the coating film, providing leveling property by thickening action, stabilizing the dispersing component, and improving barrier property.
  • the resin component (C) which has such functions and properties include, for example, vinyl resins, acrylic resins, epoxy resins, urethane resins, phenolic resins, cellulose derivatives, polymaleic acid, polyolefin, and polyester.
  • the resin component (C) used herein is not particularly limited as long as the component has a film formation property, but is typically supplied in a water-soluble or water-dispersion state. These may be used singly, or two or more thereof may be combined.
  • the solid content mass ratio (C)/ ⁇ (A) + (B) ⁇ of the resin component (C) to the silicate (A) and the inorganic salt (B) is preferably 0.01 to 3, and more preferably 0.1 to 1.5.
  • the ratio of less than 0.01 may fail to provide binder action, improve the adhesion between the base material and the coating film, provide the leveling property by thickening action, stabilize the dispersing component, improve the barrier property, or the like as expected for the resin component (C), whereas in the case of the ratio in excess of 3, the amount of the silicate and inorganic salt may be relatively reduced, thereby making it impossible to sufficiently exhibit high corrosion resistance and workability.
  • the lubricant (D) itself has lubricity and causes slippage, and has the function of reducing a frictional force between a die for processing and a material to be processed.
  • the increased frictional force during plastic working increases the working energy, generates heat, causes seizure, or the like, but when the water-based lubricating coating agent according to the present invention includes the lubricant (D), the increase in frictional force will be suppressed.
  • Examples of the lubricant (D) which has such functions and properties include waxes, polytetrafluoroethylene, fatty acid soaps, fatty acid metal soaps, fatty acid amides, molybdenum disulfide, tungsten disulfide, graphite, melamine cyanurate, amino acid compounds of layered structure, and layered clay minerals.
  • the waxes, polytetrafluoroethylene, fatty acid soaps, fatty acid metal soaps, fatty acid amides, melamine cyanurate, amino acid compounds of layered structure, and layered clay minerals are preferably blended from the perspective of corrosion resistance and liquid stability. These may be used singly, or two or more thereof may be combined.
  • specific examples of the waxes include a polyethylene wax, a paraffin wax, a microcrystalline wax, a polypropylene wax, and a carnauba wax.
  • specific examples of the fatty acid soaps include, sodium myristate, potassium myristate, sodium palmitate, potassium palmitate, sodium stearate, and potassium stearate.
  • specific examples of the fatty acid metal soaps include calcium stearate, zinc stearate, barium stearate, magnesium stearate, and lithium stearate.
  • the fatty acid amides refer to amide compound having two fatty acids, and specific examples thereof include ethylenebislauric acid amide, ethylenebisstearic acid amide, ethylenebisbehenic acid amide, N-N'-distearyladipic acid amide, ethylenebisoleic acid amide, ethylenebiserucic acid amide, hexamethylenebisoleic acid amide, and N-N'-dioleyladipic acid amide.
  • the amino acid compounds of layered structure refer to amino acids including a hydrocarbon group having 11 or more carbon atoms in a molecular structure, or derivatives thereof.
  • the layered clay minerals include natural products or synthetic products of a smectite group, a vermiculite group, a mica group, a brittle mica group, a pyrophyllite group, and a kaolinite group.
  • More specific examples thereof include montmorillonite, beidellite, nontronite, saponite, iron saponite, hectorite, sauconite, and stevensite as the smectite group, divermiculite and trivermiculite as the vermiculite group, muscovite, palagonite, illite, phlogopite, biotite, and lepidolite, as the mica group, margarite and clintonite as the brittle mica group, pyrophyllite and talc as the pyrophyllite group, and kaolinite, dickite, nacrite, halloysite, chrysotile, lizardite, and antigorite as the kaolinite group.
  • these layered clay minerals may be subjected to an organic treatment, thereby introducing an organic denaturant between layers.
  • the organic treatment is carried out in accordance with a method of introducing the organic denaturant with the interlayer distance increased by causing the layered clay minerals to swell with water.
  • the organic denaturant is an alkylamine or an alkyl quaternary ammonium salt which adsorbs in between layers to form a strong bond, and specific examples thereof include stearyldimethylamine, distearylamine, distearyldimethylamine, stearyltrimethylammoniumchloride, and distearyldimethylammoniumchloride.
  • the blend ratio of the lubricant (D) will be described for the water-based lubricating coating agent according to the present invention.
  • the solid content mass ratio (D)/ ⁇ (A) + (B) ⁇ of the lubricant (D) to the silicate (A) and the inorganic salt (B) preferably falls within the range of 0.01 to 6, and more preferably within the range of 0.1 to 2.
  • the ratio (D)/ ⁇ (A) + (B) ⁇ of less than 0.01 results in failure to sufficiently exert the friction-reducing effect expected for the lubricant (D), whereas in the case of the ratio in excess of 6, the relatively decreased amount of the silicate (A) and inorganic salt (B) may make it impossible to sufficiently exhibit high corrosion resistance and workability.
  • a viscosity modifier can be blended for the purpose of providing leveling property and thixotropy in order to ensure an evenly applied state when the lubricant is applied to the base material. It is to be noted that the blending amount is preferably 0.1 to 50 mass% with respect to the total solid content mass.
  • viscosity modifier examples include smectite clay minerals such as montmorillonite, sauconite, beidellite, hectorite, nontronite, saponite, iron saponite, and stevensite, and inorganic thickeners such as finely divided silica, bentonite, and kaolin.
  • the water-based lubricating coating agent according to the present invention can provide high corrosion resistance before and after processing, and for the purpose of further improving the corrosion resistance, other water-soluble rust inhibitors and inhibitors may be blended.
  • known inhibitors can be used, such as various types of organic acids, e.g., oleic acid, dimer acid, tartaric acid, citric acid, various types of chelating agents, e.g., EDTA, NTA, HEDTA, DTPA, mixed components of alkanolamines such as triethanolamine, amine salts and the like of p-t-butyl benzoic acid, amine salts of carboxylic acids, diacid amine bases, and combination uses of alkenyl succinic acid and water-soluble salts thereof with aminotetrazole and water-soluble salts thereof. Further, these may be used singly, or two or more thereof may be combined.
  • the blending amount is preferably 0.1 to 30 mass% with respect to the total solid content mass.
  • the liquid medium (solvent, dispersion medium) in the water-based lubricating coating agent according to the present invention is water. Further, an alcohol that is lower in boiling point than water may be blended for reducing the time period of drying the lubricant in a drying step.
  • the water-based lubricating coating agent according to the present invention may contain a water-soluble strongly alkaline component for enhancing the liquid stability.
  • a water-soluble strongly alkaline component for enhancing the liquid stability.
  • Specific examples include lithium hydroxide, sodium hydroxide, and potassium hydroxide. These may be used singly, or two or more thereof may be combined.
  • the blending amount is preferably 0.01 to 10 mass% with respect to the total solid content mass.
  • the additive amounts of components other than the components (A), (B), (C), and (D) preferably do not exceed 50 mass% of the solid content in the water-based lubricating coating agent, to the extent that required performance is not degraded.
  • the total of the additive amounts of the components (A), (B), (C), and (D) is preferably 50 mass% or more, more preferably 70 mass% or more, and further preferably 85 mass% or more on the basis of the solid content of the water-based lubricating coating agent.
  • the water-based lubricating coating agent according to the present invention is manufactured by, for example, adding and mixing the silicate (A) and the inorganic salt (B), further the resin component (C) and the lubricant (D), etc., to and with water as a liquid medium.
  • the mixing is carried out by a general method such as propeller stirring or a homogenizer.
  • the water-based lubricating coating agent according to the present invention is preferably intended for plastic working in a cold working range, such as forging, wire drawing, tube drawing, roll forming, and pressing.
  • the water-based lubricating coating agent according to the present invention is applied to metal materials such as iron or steel, stainless steel, copper or a copper alloy, aluminum or an aluminum alloy, and titanium or a titanium alloy.
  • metal materials such as iron or steel, stainless steel, copper or a copper alloy, aluminum or an aluminum alloy, and titanium or a titanium alloy.
  • the shape of the metal material is not particularly limited, but the agent is applied to not only materials such as rod materials and block materials, but also forging products (e.g., gears and shafts).
  • the water-based lubricating coating agent according to the present invention can be also used as a base coating agent for other wet lubricants or dry lubricants.
  • the use thereof as a base coating film can raise the level of workability and corrosion resistance of other wet lubricants and dry lubricants.
  • the types of lubricants combined are not particularly limited, but for example, common water-based lubricating coating agents as typified by Patent Literatures 1 to 4 mentioned above, lime soaps, and forging oils can be used as the wet lubricants.
  • such typical lubricating powders and wire drawing powders that contain, as their main constituents, a higher fatty acid soap, borax, lime, molybdenum disulfide, or the like can be used as the dry lubricants.
  • the present method for the use includes a step of cleaning a metal material, a step of applying a water-based lubricating coating agent, and a drying step.
  • the metal material to be used and the respective steps will be described below.
  • At least one cleaning treatment selected from the group consisting of shot blasting, sand blasting, wet blasting, peeling, alkali degreasing, and acid cleaning is preferably carried out before forming a water-based lubricating coating film on a metal material.
  • the cleaning herein is intended to remove oxidized scale grown by annealing or the like and various types of contamination (such as oils).
  • the step of applying the water-based lubricating coating agent according to the present invention to a metal material is not to be considered particularly limited, but a dipping method, a flow coating method, a spray method, and the like can be used.
  • the time period for the application is not particularly limited as long as the metal surface is sufficiently covered with the water-based lubricating coating agent according to the present invention by the application.
  • the metal material may be warmed to 60 to 80°C, and brought into contact with the water-based lubricating coating agent for plastic working of metal materials, or may be brought into contact with the water-based lubricating coating agent for plastic working of metal materials, which is warmed to 40 to 70°C.
  • the drying performance may be significantly improved to make drying possible at ordinary temperature, and the loss of thermal energy can be also reduced.
  • the coating weight of the water-based lubricating coating film formed on the metal surface is appropriately controlled depending on the degree of processing to be done subsequently, but the coating weight preferably falls within the range of 0.5 to 40 g/m 2 , more preferably 2 to 20 g/m 2 .
  • the coating weight is less than 0.5 g/m 2 , the lubricity is insufficient.
  • the coating weight in excess of 40 g/m 2 is not preferred because mold clogging with residues or the like is caused although there is no problem with lubricity.
  • the coating weight can be calculated from the mass difference of the metal material between before and after processing and the surface area.
  • the solid content mass (concentration) of the water-based lubricating coating agent is appropriately adjusted.
  • the intended coating weight is obtained by creating a high concentration of water-based lubricating coating agent, and diluting the agent with water.
  • the water for the adjustment by dilution is not particularly limited, but preferably deionized water or distilled water.
  • the step is not to be considered particularly limited, but preferably carried out for approximately 1 to 30 minutes at 60 to 150°C.
  • the water-based lubricating coating agent according to the present invention can prevent seizure between a mold and a material to be processed in the case of processing, and provide high corrosion resistance before and after the processing, and a base coating treatment may be carried out for the purpose of further improving workability and corrosion resistance.
  • the base coating treatment may be intended for a reactive-type coating film or a non-reactive-type coating film.
  • the reactive-type coating film include phosphates, iron oxide, zirconium oxide, zirconium hydroxide, molybdates, oxalates, and tannic acid.
  • Specific examples of the non-reactive-type coating film include silicates, borates, zirconium compounds, vanadium compounds, colloidal silica, and resin coating films.
  • the lubricating coating film formed from the water-based lubricating coating agent according to the present invention is able to be removed by dipping the film in a water-based alkaline cleaner or spray cleaning.
  • the alkaline cleaner is a liquid of a typical alkaline component such as sodium hydroxide or potassium hydroxide dissolved in water, and when the water-based lubricating coating film is brought into with the cleaner, the water-based lubricating coating film is dissolved in the cleaner, thus making it possible to remove the coating film easily. Therefore, defective plating and defective peeling of oxidized scale can be prevented without contamination in the subsequent steps due to defective film removal in the alkali cleaning.
  • Water-based lubricating coating agents according to Examples 1 to 16 and Comparative Examples 1 to 8 were prepared by adopting the respective components listed below in combinations and proportions as shown in Tables 1 to 2. It is to be noted that Comparative Example 9 corresponds to a phosphate/soap treatment.
  • Examples 1 to 16 and Comparative Examples 1 to 9 were evaluated for workability by a spike test.
  • the spike test was carried out according to the method described in JP H5-7969 A .
  • the lubricity was evaluated with the spike height after the test and the forming load. The lubricity is better as the spike height is larger, and as the forming load is lower. Further, according to the publication, the area enlargement ratio in the spike test is supposed to be approximately 10 times.
  • the lubricity of the coating film was evaluated by measuring the load at working and the spike height.
  • Spike Performance Spike Height mm / Working Load kNf ⁇ 100
  • the lubricity is more favorable as the value is larger.
  • Examples 1 to 16 and Comparative Examples 1 to 9 were evaluated for workability by an upsetting-ball ironing tribo-test.
  • the upsetting-ball ironing tribo-test was carried out according to the method described in JP 2013-215773 A .
  • the area enlargement ratio in the upsetting-ball ironing tribo-test is supposed to be 150 times or more at a maximum, and the test has a higher area enlargement ratio and reproduces stronger working as compared with the spike test mentioned above.
  • the seizure resistance of the coating film in strong working was evaluated by evaluating the amount of seizure generated at the ironing surface.
  • Fig. 1 shows indications of the evaluation.
  • Examples 1 to 16 and Comparative Examples 1 to 8 were subjected to a film removability test. It is to be noted that Comparative Example 9 was excluded from the test standard, because of the difference in typical film removal method.
  • a columnar test specimen was subjected to upsetting at a compressibility of 50% with the use of both upper and lower planar molds, and then immersed in an alkaline cleaner to remove the coating film. After the (d) water rinsing in the step (1-2), the (f) drying was carried out, and the mass of the test specimen was measured after cooling. Thereafter, after the (e) lubricating treatment, the (f) drying was carried out, and the mass of the test specimen was measured after cooling.
  • the mass of a coating film was obtained by the conversion from the mass difference between before and after the test. After the alkali cleaning, the (f) drying was carried out, and the mass of the test specimen was measured after cooling. The mass of coating film after the degreasing treatment was obtained by the conversion from the mass after the alkali cleaning and the mass after acid cleaning.
  • the film removal is more preferable as the film residual ratio is lower.
  • Examples 1 to 16 and Comparative Examples 1 to 9 were subjected to a corrosion resistance test.
  • Five test specimens were simultaneously subjected to a lubricating treatment with the use of a barrel, and the test specimens were exposed to indoors for 3 months in an open atmosphere in summer, thereby observing the degree of rust. It has been determined that the corrosion resistance is more inferior as the rusted area is larger. All of the five test specimens were evaluated.
  • Tables 4 and 5 show details of the corrosion resistance test.
  • Table 5 shows details of the corrosion resistance test.
  • the examples have achieved favorable workability (spike test, ball ironing test), film removal, and corrosion resistance (indoor exposure).
  • the blend with the sodium tungstate tends to have a favorable level, and also varies less in performance.
  • Comparative Examples 1 to 8 where the ratios of the silicate (A) and the inorganic salt (B) fall outside the scope of the claims, tend to create inferior results in the ball ironing test and the corrosion resistance test.
  • the phosphate coating film according to Comparative Example 9 subjected to the reactive soap treatment, demonstrates relatively great performance, but inferior performance as compared with the examples.
  • present invention will be further specifically described below along with advantageous effects thereof by providing examples of the present invention along with comparative examples, for the case of using the present invention as base coating films for dry lubricants and wet lubricants. It is to be noted that the present invention is not to be considered limited by these examples.
  • Water-based lubricating coating agents according to Examples 17 to 42 and Comparative Examples 11 to 18 and 20 to 27 were prepared by adopting the respective components mentioned above in combinations and proportions as shown in Tables 6 and 7.
  • Comparative Example 10 only wire drawing powder was used without any lubricating coating film according to the present invention.
  • Comparative Example 19 a lime soap was used without any lubricating coating film according to the present invention.
  • Comparative Example 28 corresponds to a phosphate/soap treatment. It is to be noted that there is no wire drawing powder used for Examples 30 to 42 and Comparative Examples 19 to 28.
  • Examples 17 to 42 and Comparative Examples 10 to 28 were evaluated for workability by a wire drawing test.
  • Wire drawing was carried out by drawing a steel wire of ⁇ 3.2 mm through a die of ⁇ 2.76.
  • Missile C40 from Matsuura Industry Co., Ltd. was used as a dry lubricant.
  • the dry lubricant was put in a die box immediately before drawing the material so as to naturally adhere to the material.
  • the evaluation was made from seizure of the test material and the residual amount of the lubrication film after the wire drawing. It is to be noted that the coating amount after the wire drawing was obtained from the mass difference between before and after removal by removing the coating film with the use of the following film remover.
  • the coating amount before working includes no lubricating powder.
  • the coating amount after working includes the lubricating powder.
  • Examples 17 to 42 and Comparative Examples 10 to 28 were evaluated for corrosion resistance.
  • the wire rod subjected to the wire drawing test mentioned above was exposed to indoors for 3 months in an open atmosphere in summer, thereby observing the degree of rust. It has been determined that the corrosion resistance is more inferior as the rusted area is larger.
  • the use of the water-based lubricant according to the present invention can achieve a balance between high workability and corrosion resistance. Furthermore, the lubricating coating film after the processing with the cleaner is also favorably removed. Accordingly, the present invention has an extremely great deal of potential in industry.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)
  • Paints Or Removers (AREA)
  • Metal Extraction Processes (AREA)
EP15768354.1A 2014-03-28 2015-03-20 Wässriges schmierbeschichtungsmittel mit ausgezeichneter korrosionsbeständigkeit und bearbeitbarkeit sowie metallmaterial Active EP3124582B1 (de)

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JP2014068039 2014-03-28
PCT/JP2015/058425 WO2015146818A1 (ja) 2014-03-28 2015-03-20 耐食性、加工性に優れた水系潤滑皮膜処理剤及び金属材料

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CN110295078A (zh) * 2019-07-18 2019-10-01 南京理工大学 一种功能石墨烯/蒙脱土/改性硫化钼润滑油添加剂

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CN108441852A (zh) * 2018-03-20 2018-08-24 鹏驰五金制品（昆山）有限公司 一种线材表面皮膜处理方法
CN109943407A (zh) * 2019-04-10 2019-06-28 上海福岛新材料科技有限公司 一种环保锻造用石墨脱模剂
KR102326485B1 (ko) * 2020-02-03 2021-11-17 한전원자력연료 주식회사 냉간 필거용 내면 윤활제 조성물

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CN110295078A (zh) * 2019-07-18 2019-10-01 南京理工大学 一种功能石墨烯/蒙脱土/改性硫化钼润滑油添加剂
CN110295078B (zh) * 2019-07-18 2021-10-08 南京理工大学 一种功能石墨烯/蒙脱土/改性硫化钼润滑油添加剂

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EP3124582A4 (de) 2017-12-13
JP6243515B2 (ja) 2017-12-06
WO2015146818A1 (ja) 2015-10-01
US20170137741A1 (en) 2017-05-18
CN105899650A (zh) 2016-08-24
CN105899650B (zh) 2020-02-21
ES2928160T3 (es) 2022-11-15
JPWO2015146818A1 (ja) 2017-04-13
EP3124582B1 (de) 2022-09-07
MX2016012566A (es) 2016-12-14

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