WO2015146818A1 - 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 - Google Patents

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 Download PDF

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WO2015146818A1
WO2015146818A1 PCT/JP2015/058425 JP2015058425W WO2015146818A1 WO 2015146818 A1 WO2015146818 A1 WO 2015146818A1 JP 2015058425 W JP2015058425 W JP 2015058425W WO 2015146818 A1 WO2015146818 A1 WO 2015146818A1
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Prior art keywords
water
film
lubricant
lubricating film
agent
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PCT/JP2015/058425
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English (en)
French (fr)
Japanese (ja)
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豪 畠山
小見山　忍
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日本パーカライジング株式会社
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Application filed by 日本パーカライジング株式会社 filed Critical 日本パーカライジング株式会社
Priority to CN201580004211.5A priority Critical patent/CN105899650B/zh
Priority to EP15768354.1A priority patent/EP3124582B1/en
Priority to US15/128,671 priority patent/US20170137741A1/en
Priority to JP2016510293A priority patent/JP6243515B2/ja
Priority to MX2016012566A priority patent/MX2016012566A/es
Priority to ES15768354T priority patent/ES2928160T3/es
Publication of WO2015146818A1 publication Critical patent/WO2015146818A1/ja

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    • 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
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    • 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
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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 film treatment agent applied when plastic processing is performed on various metal materials, and a metal material in which the treatment agent is applied on a metal material surface and dried to form a film.
  • a so-called chemical conversion coating that is a composite coating using a phosphate coating and soap is generally used.
  • chemical conversion coatings have problems such as by-products associated with reaction with metal materials, waste water treatment such as washing water, and a long treatment space.
  • water-based coating type one-component lubricants that are environmentally friendly. Has been developed.
  • Patent Document 1 discloses a composition in which (A) a water-soluble inorganic salt and (B) wax are dissolved or dispersed in water, and the solid content mass ratio (B) / (A) is 0.3 to 1.5.
  • An aqueous lubricating film treating agent for plastic working of metal materials and a method for forming the film are disclosed, which are within the range.
  • Patent Document 2 discloses a water-based lubricating film treating agent containing an alkali metal borate (A), wherein the alkali metal borate (A) contains lithium borate, and the total alkali in the alkali metal borate (A).
  • the molar ratio of lithium to metal is 0.1 to 1.0, and the molar ratio (B / M) of boric acid B and alkali metal M of alkali metal borate (A) is 1.5 to
  • This technique is said to be able to form a film having not only workability but also high corrosion resistance by suppressing the crystallization of the film that occurs when the film absorbs moisture.
  • Patent Document 3 contains an A component: an inorganic solid lubricant, a B component: a wax, and a C component: a water-soluble inorganic metal salt, and a solid content mass ratio between the A component and the B component (A component / B Component) is 0.1 to 5, and the solid content mass ratio of the C component to the total amount of the A component, the B component, and the C component (C component / (A component + B component + C component)) is 1 to 30%.
  • a water-soluble lubricant for non-phosphorous plastic working which is characterized in that. This technique is a lubricant that does not contain phosphorus, and is said to be able to realize corrosion resistance equivalent to that of a chemical conversion coating.
  • Patent Document 4 contains a water-soluble inorganic salt (A), a lubricant (B) selected from molybdenum disulfide and graphite, and a wax (C), and these are dissolved or dispersed in water.
  • (B) / (A) is a solid content weight ratio of 1.0 to 5.0
  • (C) / (A) is a solid content weight ratio of 0.1 to 1.0.
  • a method for forming the film is disclosed. This technology is said to be able to realize high workability equivalent to that of a chemical conversion treatment film by blending molybdenum disulfide or graphite with a conventional water-based lubricating film treatment agent.
  • the present inventors have formed a film in which a water-soluble silicate and a specific water-soluble inorganic salt are combined at a specific ratio, thereby forming these components.
  • the present inventors have found that high corrosion resistance (particularly long-term rust prevention), workability and sufficient film-removability, which could never be achieved by a simple substance, can be obtained.
  • the present invention (1) comprises a water-soluble silicate (A) and at least one water-soluble inorganic salt (B) selected from the group consisting of tungstate, phosphate and borate, A water-based lubricating film treating agent, wherein the mass ratio (B) / (A) is blended in a range of 0.7 to 25.
  • A water-soluble silicate
  • B water-soluble inorganic salt
  • the present invention (2) includes the resin component (C), and the solid content mass ratio thereof is (C) / ⁇ (A) + (B) ⁇ being 0.01 to 3, 1) A water-based lubricating film treating agent.
  • the resin component (C) is at least one selected from the group consisting of vinyl resins, acrylic resins, epoxy resins, urethane resins, phenol resins, cellulose derivatives, polymaleic acid, polyolefins and polyesters.
  • the water-based lubricating film treating agent of the invention (2) characterized by the above.
  • the present invention (4) includes the lubricant (D), and the solid content mass ratio thereof is (D) / ⁇ (A) + (B) ⁇ of 0.01 to 6 (1). ) To (3) water-based lubricating film treating agent.
  • the lubricant (D) is a wax, polytetrafluoroethylene, fatty acid soap, fatty acid metal soap, fatty acid amide, molybdenum disulfide, tungsten disulfide, graphite, melamine cyanurate, layered structure amino acid compound and layered
  • the water-based lubricating film treating agent of the invention (4) characterized in that it is at least one selected from the group consisting of clay minerals.
  • the water-based lubricating film treating agent for plastic working of the inventions (1) to (5) is applied and dried on the surface of the metal material so that the adhesion amount is 0.5 to 40 g / m 2 . It is a metal material that has a lubricating film and is excellent in plastic workability.
  • the water-based lubricating film treating agent of the present invention is used, a lubricating film excellent in practical corrosion resistance, workability, and film removal property can be obtained. In addition, their performance is comparable to or better than that of the chemical conversion coating, which is a great advantage over conventional water-based lubricating coatings.
  • a metal material in which the film having the above-described excellent characteristics is formed on the surface of the metal material can be obtained.
  • FIG. 1 is a standard for evaluation in the upsetting-ball ironing test (evaluation of seizure resistance).
  • Aqueous lubricant film treatment agent component or raw material, composition, etc.
  • Manufacturing method of water-based lubricant coating agent Use of water-based lubricant coating agent
  • Method of using water-based lubricant coating agent Use of water-based lubricant coating agent
  • the aqueous lubricant film treating agent of the present invention is selected from the group consisting of water-soluble silicate (A) (hereinafter referred to as silicate (A)), tungstate, phosphate and borate.
  • At least one water-soluble inorganic salt (B) (hereinafter referred to as inorganic salt (B)) is blended so that the solid content mass ratio (B) / (A) is in the range of 0.7 to 25. Do it.
  • blending in this range the film
  • water-soluble as used in the claims and the present specification means that the solubility in water at room temperature (25 ° C.) ⁇ the mass (g) of solute dissolved in 100 g of water) is at least 1 g, preferably Means 10 g or more.
  • the inorganic salt (B) is finely and uniformly incorporated into the network structure formed by the silicate (A). Become. As a result, a brittle film of silicate (A) becomes soft and processability is improved. Further, the inorganic salt (B) is incorporated into the network structure of the silicate (A), whereby the film becomes denser, the barrier property is improved, and the corrosion resistance (particularly, long-term rust prevention) is improved. Further, the film removal property is improved by moderately inhibiting the network structure of the silicate (A) by the inorganic salt (B).
  • the ratio of silicate (A) and inorganic salt (B) is important for the above performance. This performance is exhibited when the solid content mass ratio (B) / (A) is in the range of 0.7 to 25, preferably in the range of 0.9 to 10.0, and 1.1 to 3.0. If it is the range, it is more preferable.
  • (B) / (A) is less than 0.7, sufficient corrosion resistance and workability cannot be obtained, and a film having poor film removal properties is obtained. This is due to the fact that a relatively large amount of silicate forms a strong network structure.
  • (B) / (A) exceeds 25, sufficient corrosion resistance cannot be obtained, and the film has poor film adhesion and uniformity. This is because the amount of silicate is relatively small, so that a sufficient network structure cannot be constructed, the barrier property is lowered, and the adhesion and uniformity of the film are lowered.
  • silicate (A) used in the film treatment agent according to the present invention examples include lithium silicate, sodium silicate, and potassium silicate. These may be used alone or in combination of two or more. In particular, the use of lithium silicate and / or sodium silicate is preferred.
  • the inorganic salt (B) used in the film treatment agent according to the present invention will be given below.
  • the tungstate include lithium tungstate, sodium tungstate, potassium tungstate, and ammonium tungstate.
  • the phosphate include ammonium phosphate, lithium phosphate, sodium phosphate, and potassium phosphate.
  • the phosphate includes salts of condensed phosphoric acid such as tripolyphosphoric acid, metaphosphoric acid, and pyrophosphoric acid.
  • the borate include sodium borate (such as sodium tetraborate), potassium borate (such as potassium tetraborate), and ammonium borate (such as ammonium tetraborate). These may be used alone or in combination of two or more.
  • the resin component (C) is blended for the purpose of binder action, improvement in adhesion between the substrate and the film, imparting leveling property by thickening action, stabilizing the dispersion component, and improving barrier properties.
  • the resin component (C) having such functions and properties include vinyl resin, acrylic resin, epoxy resin, urethane resin, phenol resin, cellulose derivative, polymaleic acid, polyolefin, and polyester.
  • the resin component (C) used here is not particularly limited as long as it has film-forming properties, and is generally supplied in a water-soluble or water-dispersed state. These may be used alone or in combination of two or more.
  • the aqueous lubricant film treating agent has a solid content mass ratio of silicate (A), inorganic salt (B) and resin component (C) of 0.01 to 3 (C) / ⁇ (A) + (B) ⁇ . It is preferable that (C) / ⁇ (A) + (B) ⁇ is more preferably 0.1 to 1.5.
  • (C) / ⁇ (A) + (B) ⁇ is more preferably 0.1 to 1.5.
  • the binder action expected for the resin component (C), the adhesion between the base material and the film, the leveling property by the thickening action, the stabilization of the dispersion component, the improvement of the barrier property, etc. are sufficiently exhibited. In some cases, when the number exceeds 3, the amount of silicate or inorganic salt becomes relatively small, and high corrosion resistance and workability may not be sufficiently exhibited.
  • the lubricant (D) itself has lubricity and slipperiness, and has a function of reducing the frictional force between the die during processing and the workpiece. In general, when the frictional force increases during plastic processing, processing energy increases, heat generation, seizure, etc. occur. However, when the lubricant (D) is included in the aqueous lubricant coating agent of the present invention, the increase in frictional force is suppressed. It will be.
  • Examples of the lubricant (D) having such functions and properties include wax, polytetrafluoroethylene, fatty acid soap, fatty acid metal soap, fatty acid amide, molybdenum disulfide, tungsten disulfide, graphite, melamine cyanurate, layered structure
  • Examples include amino acid compounds and layered clay minerals.
  • a blend of wax, polytetrafluoroethylene, fatty acid soap, fatty acid metal soap, fatty acid amide, melamine cyanurate, layered structure amino acid compound and layered clay mineral is more preferable. These may be used alone or in combination of two or more.
  • wax examples include polyethylene wax, paraffin wax, microcrystalline wax, polypropylene wax, and carnauba wax.
  • fatty acid soaps include sodium myristate, potassium myristate, sodium palmitate, potassium palmitate, sodium stearate, and potassium stearate.
  • fatty acid metal soaps include calcium stearate, zinc stearate, barium stearate, magnesium stearate, and lithium stearate.
  • Fatty acid amide is an amide compound having two fatty acids.
  • the layered structure amino acid compound is an amino acid having a hydrocarbon group having 11 or more carbon atoms in the molecular structure or a derivative thereof.
  • a specific example is N-lauroyl-L-lysine [C 11 H 23 CONH (CH 2 ) 4 CH (NH 2 ) COOH].
  • Examples of the layered clay mineral include natural products or synthetic products of the smectite group, vermiculite group, mica group, brittle mica group, pyrophyllite group, and kaolinite group. More specifically, in the smectite group, montmorillonite, beidellite, nontronite, saponite, iron saponite, hectorite, soconite, stevensite, and vermiculite group are di. Vermiculite, tri.
  • these layered clay minerals may be subjected to organic treatment to introduce an organic modifier between the layers.
  • the organic treatment is carried out by introducing an organic modifier in a state where the lamellar clay mineral is swollen with water to increase the interlayer distance.
  • the organic modifier is an alkylamine or alkyl quaternary ammonium salt that adsorbs between layers to form a strong bond.
  • Specific examples include stearyl dimethylamine, distearylamine, distearyldimethylamine, stearyltrimethylammonium chloride, distearyldimethyl. Ammonium chloride is mentioned.
  • the blending ratio of the lubricant (D) of the water-based lubricating film treating agent according to the present invention will be described.
  • the solid content mass ratio of the silicate (A), the inorganic salt (B), and the lubricant (D) is 0.01 to (D) / ⁇ (A) + (B) ⁇ .
  • a range of 6 is preferable, and a range of 0.1 to 2 is more preferable.
  • the aqueous lubricant film treatment agent of the present invention is uniformly applied when a lubricant is applied to the substrate.
  • a viscosity modifier can be blended for the purpose of imparting leveling properties and thixotropy.
  • the blending amount of these is preferably 0.1 to 50% by mass relative to the total solid mass.
  • viscosity modifiers examples include, as a specific example, smectite clay minerals such as montmorillonite, soconite, beidellite, hectorite, nontronite, saponite, iron saponite, and stevensite, and inorganic inorganic materials such as finely divided silica, bentonite, and kaolin.
  • smectite clay minerals such as montmorillonite, soconite, beidellite, hectorite, nontronite, saponite, iron saponite, and stevensite
  • inorganic inorganic materials such as finely divided silica, bentonite, and kaolin.
  • a thickener is mentioned.
  • the water-based lubricating film treatment agent of the present invention can impart high corrosion resistance before and after processing, but may further contain other water-soluble rust preventives and inhibitors for the purpose of further improving the corrosion resistance.
  • Specific examples include various organic acids such as oleic acid, dimer acid, tartaric acid and citric acid, various chelating agents such as EDTA, NTA, HEDTA and DTPA, mixed components of alkanolamines such as triethanolamine, and pt-butylbenzoic acid.
  • Known amines such as amine salts of acids, carboxylic acid amine salts, dibasic amine bases, alkenyl succinic acid and water-soluble salts thereof, and aminotetrazole and water-soluble salts thereof can be used. These may be used alone or in combination of two or more. The blending amount of these is preferably 0.1 to 30% by mass relative to the total solid mass.
  • the liquid medium (solvent, dispersion medium) in the aqueous lubricant film treatment agent of the present invention is water.
  • an alcohol having a boiling point lower than that of water may be blended.
  • the aqueous lubricant film treatment agent of the present invention may contain a water-soluble strong alkali component in order to enhance the stability of the liquid.
  • a water-soluble strong alkali component include lithium hydroxide, sodium hydroxide, and potassium hydroxide. These may be used alone or in combination of two or more. The blending amount of these is preferably 0.01 to 10% by mass relative to the total solid mass.
  • the addition amount other than (A), (B), (C), and (D) does not exceed 50% by mass of the solid content of the water-based lubricating coating agent as long as the required performance is not lowered.
  • the total amount of addition of (A), (B), (C), and (D) is preferably 50% by mass or more, and 70% by mass or more, based on the solid content of the aqueous lubricant film. It is more preferable that it is 85 mass% or more.
  • the water-based lubricating film treating agent according to the present invention is mixed, for example, by adding a silicate (A) and an inorganic salt (B), further a resin component (C), a lubricant (D), etc. to water which is a liquid medium. It is manufactured by doing. Mixing is performed by a general method such as propeller stirring or a homogenizer.
  • the water-based lubricating film treating agent of the present invention is preferably for plastic working in the cold region such as forging, wire drawing, tube drawing, roll forming, pressing, and the like.
  • the water-based lubricating film treating agent of the present invention is applied to metal materials such as iron or steel, stainless steel, copper or copper alloy, aluminum or aluminum alloy, titanium or titanium alloy.
  • the shape of the metal material is not particularly limited, and is applicable not only to raw materials such as rods and block materials but also to forged shapes (such as gears and shafts).
  • the water-based lubricating film treating agent of the present invention can be used as a base film treating agent for other wet lubricants or dry lubricants. By using it as an undercoat, the workability and corrosion resistance of other wet lubricants and dry lubricants can be raised.
  • the type of lubricant to be combined is not particularly limited.
  • a general water-based lubricating film treatment agent represented by Patent Documents 1 to 4, lime soap, and forging oil can be used as a wet lubricant.
  • the dry lubricant for example, general lubricating powder or wire drawing powder mainly composed of higher fatty acid soap, borax, lime, molybdenum disulfide or the like can be used.
  • This method of use includes a metal material cleaning step, a water-based lubricating film treating agent application step, and a drying step.
  • the metal material and each process which are objects of use will be described.
  • ⁇ Cleaning process Before forming the water-based lubricating film on the metal material, it is preferable to perform at least one cleaning treatment selected from the group consisting of shot blasting, sand blasting, wet blasting, peeling, alkali degreasing, and acid cleaning.
  • the purpose of cleaning is to remove oxide scales and various types of dirt (oil, etc.) grown by annealing or the like.
  • the process of applying the water-based lubricating film of the present invention to a metal material is not particularly limited, but an immersion method, a flow coating method, a spray method, or the like can be used. Application is not limited as long as the metal surface is sufficiently covered with the water-based lubricating film treating agent of the present invention.
  • the metal material may be heated to 60 to 80 ° C. and brought into contact with the metal-based plastic working water-based lubricant coating agent, or the metal material plastic working water system heated to 40 to 70 ° C. A lubricant film treatment agent may be contacted.
  • the adhesion amount of the water-based lubricating film formed on the metal surface is appropriately controlled depending on the degree of subsequent processing, but the adhesion amount is preferably in the range of 0.5 to 40 g / m 2 , more preferably 2 It is in the range of ⁇ 20 g / m 2 .
  • the adhesion amount is less than 0.5 g / m 2 , the lubricity is insufficient.
  • the adhesion amount exceeds 40 g / m 2 , there is no problem in lubricity, but clogging of the mold and the like are not preferable.
  • the amount of adhesion can be calculated from the mass difference and surface area of the metal material before and after the treatment.
  • the solid content mass (concentration) of the water-based lubricating film treating agent is appropriately adjusted.
  • a high concentration aqueous lubricant film is prepared and diluted with water to obtain the desired amount of adhesion.
  • the water to be diluted is not particularly limited, but deionized water and distilled water are preferable.
  • the drying step is preferably carried out at 60 to 150 ° C for about 1 to 30 minutes.
  • the water-based lubricating film treating agent of the present invention prevents seizure between the mold and the workpiece during processing and can impart high corrosion resistance before and after processing, but for the purpose of further improving workability and corrosion resistance.
  • An undercoat treatment may be performed.
  • the base film treatment may be a reactive film or a non-reactive film.
  • Specific examples of the reactive coating include phosphate, iron oxide, zirconium oxide, zirconium hydroxide, molybdate, oxalate, and tannic acid.
  • Specific examples of the non-reactive film include silicate, borate, zirconium compound, vanadium compound, colloidal silica, and resin coating film.
  • the lubricating film formed by the water-based lubricating film treating agent of the present invention can be removed by immersing in a water-based alkaline cleaning agent or by spray cleaning.
  • An alkaline cleaner is a solution in which common alkaline components such as sodium hydroxide and potassium hydroxide are dissolved in water.
  • an aqueous lubricant film is brought into contact with this, the aqueous lubricant film dissolves in the cleaning solution, so that The film can be removed. Therefore, there is no contamination in the subsequent process due to defective film removal by alkali cleaning, and plating defects and oxide scale peeling defects can be prevented in advance.
  • the area expansion rate is 150 times or more at maximum, and the area expansion rate is very large compared to the spike test described above, and this is a test that reproduces strong machining.
  • Test piece for evaluation S10C spheroidized annealing material 14 mm ⁇ ⁇ 32 mm Bearing ball: 10mm ⁇ SUJ2 Evaluation criteria: It was evaluated how much area burned with respect to the entire area of the ironing surface. The standard of evaluation is shown in FIG.
  • step (d) after washing with water, (f) was dried, and after cooling, the mass of the test piece was measured. Thereafter, (e) after the lubrication treatment, (f) was dried and the mass of the test piece was measured after cooling. The film mass was converted by the mass difference before and after that. After washing with alkali (f), drying was performed, and the mass of the test piece was measured after cooling. The film mass after degreasing treatment was converted from the mass after alkali washing and the mass after pickling.
  • test pieces were lubricated at the same time, and the test pieces were exposed indoors in an open atmosphere in summer for 3 months to observe the occurrence of rust. It was judged that the larger the rusting area, the lower the corrosion resistance. Evaluation was carried out on all five test pieces.
  • Test piece for evaluation S45C spheroidized annealing material 25 mm ⁇ ⁇ 30 mm Evaluation criteria: A: Rust area 3% or less (remarkably superior to phosphate / soap film) ⁇ : Rust area over 3%, 10% or less (better than phosphate / soap film) ⁇ : Rust area over 10%, 20% or less (equivalent to phosphate / soap film) ⁇ : Rust area over 20%, 30% or less (inferior to phosphate / soap film) ⁇ : Rust area more than 30% (remarkably inferior to phosphate / soap film) (1-3-5) Overall score evaluation The above four evaluation results were scored according to the criteria shown in Table 3, and the total score was summarized.
  • Tables 4 and 5 show the details of the corrosion resistance test. As is apparent from the table, the examples had good workability (spike test, ball ironing test), film removal property, and corrosion resistance (indoor exposure). Moreover, regarding the corrosion resistance, the level of blending sodium tungstate tended to be good, and the performance variation was small. In Comparative Examples 1 to 8, the ratio of the silicate (A) to the inorganic salt (B) was outside the scope of the present invention, but the results of the ball ironing test and the corrosion resistance test tended to be inferior. What performed the reaction soap process to the phosphate membrane
  • Example B the case where the present invention is used as an undercoat of a dry lubricant and a wet lubricant will be described more specifically together with the effects of the present invention by giving examples of the present invention together with comparative examples. In addition, this invention is not restrict
  • Example B
  • Lubrication treatment ⁇ Lubrication treatment of Examples 17 to 28 and Comparative Examples 11 to 18> Processed by standard steps as described in (1-2).
  • E Lubricant film treatment: Water-based lubricant film treatment agent produced in (2-1) Temperature 60 ° C., immersion 1 minute ⁇ Pretreatment and film treatment of Examples 30 to 41 and Comparative Examples 20 to 27> Processed by standard steps as described in (1-2).
  • the amount of the film after wire drawing was determined from the difference in mass before and after the film was peeled off using the following film peeling agent.
  • Test piece for evaluation SWCH45K material ⁇ 3.2 mm ⁇ 20 m Die diameter: ⁇ 2.76
  • Film stripper Commercially available alkaline stripper (FC-E6463, manufactured by Nihon Parkerizing Co., Ltd.), 20 g / L Film removal conditions: liquid temperature 60 ° C., immersion time 2 minutes
  • Evaluation criteria: Film residual ratio (%) (film amount before processing / film amount after processing) ⁇ 100 *
  • the amount of coating before processing does not include lubricating powder.
  • the coating amount after processing includes lubricating powder.
  • Evaluation criteria A: Remarkably superior to phosphate / soap film (rust area 3% or less) ⁇ : Superior to phosphate / soap film (rust area 3% or more, less than 10%) ⁇ : Same as phosphate / soap film (rust area 10% or more, less than 20%) ⁇ : Inferior to phosphate / soap film (rust area 20% or more, less than 30%) X: Remarkably inferior to phosphate / soap film (rust area 30% or more)
  • Table 8 shows the test results. In all of the examples, a lot of film remained, and the workability and corrosion resistance were good. From the fact that the corrosion resistance after wire drawing is also high, it can be seen that a large amount of the lubricating film of the present invention remains after processing. Comparative Examples 10 and 19 were at a level where the lubricant of the present invention was not used, but the wire drawability and corrosion resistance were greatly inferior. In Comparative Examples 11 to 18 and 20 to 27, the ratio of the silicate (A) to the inorganic salt (B) was set inappropriately, but the film remaining amount after wire drawing and the corrosion resistance were inferior.
  • the sample obtained by subjecting the phosphate film of Comparative Example 28 to reactive soap treatment has excellent performance, but wastewater treatment and liquid management are required, and it cannot be used in simple treatment processes or equipment. This creates a large environmental impact.

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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)
PCT/JP2015/058425 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 WO2015146818A1 (ja)

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CN201580004211.5A CN105899650B (zh) 2014-03-28 2015-03-20 耐腐蚀性、加工性优异的水系润滑皮膜处理剂及金属材料
EP15768354.1A EP3124582B1 (en) 2014-03-28 2015-03-20 Aqueous lubricating coating agent having excellent corrosion resistance and workability, and metal material
US15/128,671 US20170137741A1 (en) 2014-03-28 2015-03-20 Water-based lubricating coating agent with excellent corrosion resistance and workability, and metal material
JP2016510293A JP6243515B2 (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
MX2016012566A MX2016012566A (es) 2014-03-28 2015-03-20 Agente de revestimiento lubricante a base de agua con excelente resistencia a la corrosion y manejabilidad, y material metalico.
ES15768354T ES2928160T3 (es) 2014-03-28 2015-03-20 Agente de recubrimiento lubricante acuoso que tiene resistencia a la corrosión y trabajabilidad excelentes, y material metálico

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

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