JP2006143988A - Lubricating coating film for plastic processing, composition for forming the same, material for producing plastic processed article and method for producing metal tube, metal wire or metal stick - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a lubricating coating film for plastic processing, which is excellent in adhesiveness and lubricating property, a composition for forming a lubricating coating film for plastic processing and a material for plastic processing, a method for producing a plastic processed article, and a method for producing a metal tube, a metal wire or a metal stick, the methods requiring no under-coating by a chemical treatment and being capable of conducting by simple process steps. <P>SOLUTION: The lubricating coating film for plastic processing comprises a resin layer formed on a surface of a base material. The resin layer contains wax and also contains 25-99 wt% of a resin showing a glass transition temperature of 30°C or lower under 100 wt% of the resin layer, such as one or more of a (meth)acrylate resin, a urethane resin, a polyester resin, a vinyl alcohol resin, a polyamide resin and a fluorocarbon resin. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a lubricating film for plastic working, a composition for forming a lubricating film for plastic working, a raw material for plastic working, a method for producing a plastic processed product, and a method for producing a metal tube, a metal wire, or a metal rod. More specifically, in cold plastic working of metal, a lubricating film with high adhesion is formed on the surface of the metal or mold as the work material to exert excellent lubricity, thereby reducing the processing power by reducing friction. By forming a lubricating film for plastic working, a composition for forming a lubricating film for plastic working, and forming a lubricating film for plastic working, which can realize an increase in the life of rolls and tools and an improvement in product quality by suppressing wear and seizure. The present invention relates to a plastic working material used for manufacturing a processed product, a method of manufacturing a plastic processed product using the plastic processing material, and a manufacturing method of a metal tube, a metal wire, or a metal bar.

  Examples of cold plastic working of metal include plate rolling, tube rolling, steel bar (section steel, bar wire, wire rod) rolling, drawing, forging, shearing, press molding and the like. Examples of the metal subjected to plastic working as a workpiece include various steels such as carbon steel and stainless steel, aluminum, copper, titanium, and alloys thereof, and multilayer clads thereof.

  Generally, in plastic processing of a metal material, a liquid or solid lubricant is used for the purpose of reducing friction caused by metal contact between a workpiece and a tool and preventing seizure and galling. Usually, the lubrication method in cold plastic working is the material, processing method, surface pressure, processing speed, surface roughness of the material to be rolled and the roll or tool (hereinafter referred to as “tool”). It is used properly according to the degree and working environment. The lubrication process can be roughly divided into two. One is a lubrication treatment in which the lubricant is physically attached to the metal surface, and the other is a lubrication treatment in which a lubricant film is adhered after the carrier film is formed on the metal surface by a chemical reaction.

  The lubrication treatment in which a carrier film is generated on a metal surface by a chemical reaction and then a lubricant is attached is called a so-called chemical film treatment. Such a chemical conversion film treatment is performed by forming a coating film such as a phosphate having a role as a carrier on the surface of a workpiece by a chemical reaction, and then reacting soap or non-reacting soap such as sodium stearate or calcium stearate as a lubricant. Etc. are performed. The film formed by such a chemical conversion film treatment has a two-layer structure of a chemical conversion film as a carrier and a lubricant, and exhibits very high seizure resistance. Therefore, such a chemical conversion film treatment has been used in a very wide range in the field of plastic working such as wire drawing, pipe drawing and forging. However, since the chemical conversion film treatment is a chemical reaction, it is difficult to treat a workpiece having poor chemical reactivity, and complex liquid management is also required for a treatable workpiece. Further, as shown in FIG. 1 (A), in order to apply a lubricant on the formed chemical conversion film, a number of processing steps are required including water washing and pickling. Furthermore, a large amount of waste liquid comes out from the washing water and chemical conversion coating used in the treatment, and heating is necessary to control the chemical reaction. There's a problem.

  In order to solve the problems of the chemical conversion film treatment, a lubrication treatment in which the aforementioned lubricant is physically attached to the metal surface has been studied. As a result of such studies, a method using an oil-based lubricant or a water-based lubricant has been proposed. For example, as an oil-based lubricant, the following Patent Document 1 discloses a metal soap or solid in a lubricating oil containing an extreme pressure agent such as chlorinated paraffin and phosphate ester, an isobutylene / n-butene copolymer and animals and plants. A cold work lubricant containing a lubricant is disclosed. In addition, as an aqueous lubricant, the following Patent Document 2 discloses a cold or warm processing of a metal tube, which contains a bicarbonate as a main component and a small amount of a dispersant, a surfactant and a solid lubricant added thereto. A lubricant is disclosed, and the following Patent Document 3 discloses a lubricant composition in which a water-soluble polymer or an aqueous emulsion thereof is used as a base material and a solid lubricant and a chemical film-forming agent are blended.

  Further, Patent Document 4 below includes at least one selected from water-soluble polyesters having a specific average molecular weight and water-soluble polysaccharides, at least one selected from water-soluble polyamides, and waxes having a specific melting point. There is disclosed a lubricant composition for forming a lubricating film which is composed of at least one selected and water, and each component has a specific weight ratio and which can be easily removed by washing with water. Patent Document 5 below contains a synthetic resin, a water-soluble inorganic salt, and water, the solid content weight ratio of the synthetic resin to the water-soluble inorganic salt is a specific value, and the synthetic resin is dissolved. Alternatively, a lubricant composition for plastic working of a dispersed metal material is disclosed.

Japanese Patent Publication No.4-1798 Japanese Patent Publication No. 58-30358 Japanese Patent Laid-Open No. 52-20967 Japanese Patent Laid-Open No. 6-10877 JP 2000-63880 A

  However, even the cold working lubricant disclosed in Patent Document 1 is somewhat difficult in workability as compared with the conventional lubrication method in which chemical conversion coating is performed, and the extreme pressure additive is used. Therefore, there is a problem that odor is generated during processing. The lubricant disclosed in Patent Document 2 has not yet been widely used in place of the chemical conversion coating treatment. Furthermore, the lubricant of the above-mentioned Patent Document 3 has not obtained a lubricant having lubricity comparable to the chemical conversion film treatment. As for each of the lubricants in Patent Documents 4 and 5, a lubricant having lubricity comparable to the chemical conversion coating treatment has not been obtained, and the glass transition temperature of the contained resin is not mentioned.

  The present invention does not require a base by chemical conversion treatment in cold plastic working of metal, and is excellent in forming a lubricant film with high adhesion on the surface of a metal or mold as a workpiece in a simple process. For forming lubrication coatings for plastic working and plastic working that can reduce lubrication, reduce machining power by reducing friction, extend the life of rolls and tools by suppressing wear and seizure, and improve product quality Composition, plastic working material for forming plastic working product by forming lubricating film for plastic working, method for producing plastic working product using plastic working material, and metal tube, metal wire or metal rod An object is to provide a manufacturing method.

  As described above, in general, in order for a lubricating coating made of resin to have high lubricity, both a lubricating function that imparts slipping and a protective function that protects the coating are required. In other words, in cold plastic working of metal, the surface area of the work material is rapidly expanded while being ironed on the friction surface of the work material and the tool, so that the lubricant always follows these changes. The malleable ductility covering the friction surface and the strength to withstand the pressure are required. However, it has been substantially difficult to combine these functions with a single layer of coating.

  Therefore, the present inventors examined a lubrication method using a resin-based film in order to obtain high lubricity in cold plastic working of metals. As a result, if the glass transition temperature of the resin to be included is higher than the temperature immediately after the start of plastic processing, the resin coating cannot follow the change in the friction surface immediately after the start of processing, and brittle fracture (breaks up) resulting in friction. On the other hand, if the glass transition temperature of the resin is lower than the temperature immediately after the start of plastic processing, the resin behaves as a viscous fluid, so it can follow changes in the friction surface immediately after the start of processing. Investigated. And, by using a lubricating film for plastic working containing a specific amount of resin having a specific glass transition temperature, sufficient strength can be obtained even in severe processing, without causing film breakage, and against shearing The present invention has been completed by investigating that the dispersed wax particles provide a film having a lubricating function and can reduce the frictional resistance during processing.

The present invention is as follows.
(1) A lubricating film for plastic working comprising a resin layer formed on the surface of a base material,
The resin layer contains wax particles, and the resin layer contains 25 to 99 wt% of a resin having a glass transition temperature of 30 ° C. or lower when the resin layer is 100 wt%. Lubricant coating.
(2) The plasticity according to (1), wherein the resin is at least one of (meth) acrylic resin, urethane resin, polyester resin, vinyl acetate resin, polyvinyl alcohol resin, polyamide resin, and fluorine resin. Lubricant coating for processing.
(3) The wax particles have a solid or viscosity of 10 mPa · s or higher at 100 ° C., and the content of the wax particles is 0.5 to 74.5 wt% when the resin layer is 100 wt%. The lubricating film for plastic working according to the above (1) or (2).
(4) The lubricating film for plastic working according to any one of (1) to (3), wherein the wax particles have an average particle size of 10 μm or less.
(5) The resin layer further contains at least one extreme pressure additive selected from a sulfur-based extreme pressure additive, a phosphorus-based extreme pressure additive, and a chlorine-based extreme pressure additive, and the resin layer is 100 wt%. %, The plastic coating lubricating film according to any one of the above (1) to (4), wherein the content of the extreme pressure additive is 0.5 to 74.5 wt% in terms of solid content.
(6) The lubricating film for plastic working according to any one of (1) to (5), wherein the resin layer further contains fine particles having an anti-seizure effect.
(7) When the solvent contains a resin having a glass transition temperature of 30 ° C. or lower and wax particles, and the solid content of the lubricating film forming composition for plastic working is 100 wt%, the glass A composition for forming a lubricating film for plastic working, wherein the content of a resin having a transition temperature of 30 ° C. or lower is 25 to 99 wt%.
(8) The plastic processing according to (7), wherein the resin is at least one of (meth) acrylic resin, urethane resin, polyester resin, vinyl acetate resin, polyvinyl alcohol resin, polyamide resin, and fluorine resin. Lubricating film forming composition.
(9) The lubricating film for plastic working according to the above (7), wherein the resin is cross-linked by a compound containing at least one metal element of a typical metal element and a transition metal element and / or ions thereof. Forming composition.
(10) The lubricating film for plastic working according to (7), wherein the resin is a compound containing at least one metal element of a typical metal element and a transition metal element and / or an ionomer cross-linked by an ion thereof. Forming composition.
(11) The above (9) or (9), wherein the typical metal element is at least one of alkaline earth metal, aluminum, and zinc, and the transition metal element is at least one of iron and copper. The composition for forming a lubricating film for plastic working as described in 10).
(12) The wax particles have a solid content or a viscosity of 10 mPa · s or more at 100 ° C., and the content of the wax particles when the solid content of the lubricating film forming composition for plastic working is 100 wt%. The composition for forming a lubricating film for plastic working according to any one of the above (7) to (11), wherein is 0.5 to 74.5 wt%.
(13) The composition for forming a lubricating film for plastic working according to any one of (7) to (12), wherein the wax particles have an average particle size of 10 μm or less.
(14) A composition for forming a lubricating coating for plastic working, further comprising at least one extreme pressure additive selected from a sulfur-based extreme pressure additive, a phosphorus-based extreme pressure additive, and a chlorine-based extreme pressure additive The plastic working according to any one of the above (7) to (13), wherein the content of the extreme pressure additive is 0.5 to 74.5 wt% in terms of solid content when the solid content is 100 wt% Lubricating film forming composition.
(15) The composition for forming a lubricating film for plastic working according to any one of (7) to (14), further comprising fine particles having an anti-seizure effect.
(16) The composition for forming a lubricating film for plastic working as described in (15) above, wherein the fine particles are oxides of at least one metal element of a typical metal element and a transition metal element.
(17) The typical metal element is at least one of alkaline earth metal, aluminum, and zinc, and the transition metal element is at least one of iron and copper. A composition for forming a lubricating coating for plastic working.
(18) The composition for forming a lubricating film for plastic working according to any one of (7) to (17), wherein the solvent is water or a solvent containing at least water.
(19) The plastic working lubricant film according to any one of (1) to (6) is formed on a surface of a material for producing a plastic processed product having an arbitrary shape. Material for plastic working.
(20) A method for producing a plastically processed product, comprising plastically processing the material for plastic processing described in (19) above.
(21) A method for producing a metal tube, a metal wire, or a metal rod, wherein the plastic working material according to (19) is drawn.

According to the lubricating film for plastic working of the present invention, excellent lubricity can be exhibited even under severe working conditions where seizure is likely to occur in various metal working such as plastic working of metal in the cold. In particular, compared to other processes such as pressing of steel sheets, the surface area of ironing and work materials is significantly increased, and high seizure resistance is exhibited in cold plastic processing (especially drawing) with severe processing conditions. Can do. Further, the lubricating film for plastic working of the present invention can be applied to various metals such as steel, stainless steel, “Inconel” (trade name), titanium, titanium alloy, aluminum, aluminum alloy, magnesium, magnesium alloy, copper, and copper alloy material. Can be applied.
In addition, when a specific amount of wax particles having specific characteristics at 100 ° C. is contained, in various metal processing such as cold metal plastic processing, further excellent lubrication even under severe processing conditions where seizure is likely to occur. Can demonstrate its sexuality.
Furthermore, when a specific extreme pressure additive is contained, the lubricating performance in the extreme pressure lubrication region can be further improved. Furthermore, the seizure prevention effect can be further improved.
Further, when fine particles are contained, the shear strength and adhesion strength of the coating can be improved. Furthermore, the seizure prevention effect can be further improved.

When the composition for forming a lubricating coating for plastic working of the present invention is used, a coating having excellent lubricity can be formed by a simple coating forming treatment as compared with a conventional chemical conversion coating treatment.
In addition, when a specific amount of wax particles having specific characteristics at 100 ° C. is contained, it is more excellent in lubricity even under severe processing conditions in which seizure is likely to occur in plastic processing of metals in the cold. Can be obtained.
Furthermore, when a specific extreme pressure additive is contained, a coating film having better lubricating performance in the extreme pressure lubrication region can be obtained. Furthermore, it is possible to obtain a film having a more excellent anti-seizure effect.
In addition, when fine particles are contained, a film excellent in the shear strength and adhesion strength of the film can be obtained. Furthermore, it is possible to obtain a film excellent in the seizure prevention effect.

According to the plastic working material of the present invention, good seizure resistance, formability, and workability can be exhibited during plastic working, and the metal material can be protected from contact wrinkles during conveyance.
According to the method for manufacturing a plastic processed product of the present invention and the method for manufacturing a metal tube, metal wire, or metal bar of the present invention, it is possible to suppress the occurrence of seizure, galling or the like. As a result, a processed product with excellent quality can be obtained.

The present invention will be described in detail below.
In the present invention, “(meth) acrylic” means acrylic and methacrylic, and “(meth) acrylate” means acrylate and methacrylate.

(1) Lubricating film for plastic working The lubricating film for plastic working of the present invention is a lubricating film for plastic working comprising a resin layer formed on the surface of a base material, and this resin layer has a glass transition temperature of 30 ° C. or lower. Contains resin and wax particles.

  The lubricating film for plastic working of the present invention forms a resin layer having a high protective function in which wax particles imparting slip are dispersed as a film on a base material. As a result, sufficient strength can be obtained even in severe processing, film breakage does not occur, and the coating has a lubricating function due to dispersed wax particles against shearing, thereby reducing the frictional resistance during processing. it can.

  In the present invention, the glass transition temperature of the “resin” constituting the resin layer is 30 ° C. or less, preferably 26 ° C. or less, more preferably 23 ° C. or less, more preferably 15 ° C. or less, and particularly preferably 10 ° C. or less. is there. Moreover, about the minimum of the range of the said glass transition temperature, it can set suitably, -85 degreeC is mentioned as the example. When the glass transition temperature is higher than 30 ° C., the lubricating coating cannot follow the increase in the surface area of the friction surface immediately after the start of plastic processing, and brittle fracture occurs, resulting in frequent detachment from the friction surface. The glass transition temperature can be measured by a method according to JIS K7121 or by dynamic viscoelasticity measurement. When the resin is a (meth) acrylic resin, the glass transition temperature can be calculated by the FOX equation from the glass transition temperature of the homopolymer of each ethylenically unsaturated monomer to be polymerized. The glass transition temperature can be changed by appropriately selecting the type of resin. Furthermore, it can be lowered by using a plasticizer and external plasticizing.

There is no limitation in particular in the kind of the said resin. This resin may be an uncrosslinked polymer or a crosslinked polymer. In the latter case, a compound containing at least one metal element of a typical metal element and a transition metal element and / or a resin crosslinked with ions thereof can be used. Examples of the typical metal element include alkali metals, alkaline earth metals, aluminum, and zinc. Among these, at least one of alkaline earth metal, aluminum, and zinc is preferable. Moreover, as said transition metal element, iron, copper, etc. are mentioned, for example.
Specific examples of the resin include (meth) acrylic resins, urethane resins, polyester resins, vinyl acetate resins, polyvinyl alcohol resins, polyamide resins, and fluorine resins. The resins having a glass transition temperature of 30 ° C. or lower may be used alone or in combination of two or more. By setting it as the resin layer containing this specific resin, it can be set as a film with a high lubrication function.

As long as the (meth) acrylic resin is obtained by polymerizing one or more acrylic monomers, a homopolymer or a copolymer may be used. There is no particular limitation on the structure and type. Examples of the acrylic monomer include methyl (meth) acrylate, ethyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, and octyl (meth) acrylate. Alkyl (meth) acrylate (the carbon number of the alkyl group is preferably 1-8, more preferably 1-6, particularly preferably 1-4); methoxymethyl (meth) acrylate, methoxyethyl (meth) acrylate, ethoxymethyl Lower alkoxy lower alkyl (meth) acrylates such as (meth) acrylate, ethoxyethyl (meth) acrylate, and methoxybutyl (meth) acrylate; 2-hydroxyethyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate Hydroxy lower alkyl (meth) acrylates such as acrylamide; acrylamide, methacrylamide; N-unsubstituted or substituted such as N-methylol acrylamide, N-methylol methacrylamide, N-butoxymethyl acrylamide, and N-butoxymethyl methacrylamide (particularly (Lower alkoxy substituted) (meth) acrylamide having a methylol group; Phosphonyloxy lower alkyl (meth) such as phosphonyloxymethyl (meth) acrylate, phosphonyloxyethyl (meth) acrylate, and phosphonyloxypropyl (meth) acrylate Examples thereof include acrylate; acrylonitrile; one or more of acrylic acid, methacrylic acid and the like. In addition, said lower alkoxy and said lower alkyl usually mean a C1-C5 alkoxy and alkyl, respectively, Preferably it is C1-C4, More preferably, it is 1-3.
The (meth) acrylic resin is one or more of the above acrylic monomers and one of other ethylenic monomers such as styrene, methylstyrene, vinyl acetate, vinyl chloride, vinyltoluene, and ethylene. Or a copolymer with 2 or more types may be sufficient. In that case, a copolymer containing 30 mol% or more of the unit composed of the acrylic monomer is preferable. Examples of the copolymer include a compound containing at least one metal element of a typical metal element and a transition metal element and / or an ionomer cross-linked with an ion thereof. Examples of the typical metal element include alkali metals, alkaline earth metals, aluminum, and zinc. Among these, at least one of alkaline earth metal, aluminum, and zinc is preferable. Moreover, as said transition metal element, iron, copper, etc. are mentioned, for example.

  The urethane resin is a synthetic resin having a urethane bond (-NHCOO-), and generally obtained by a polyaddition reaction of a polyisocyanate compound having two or more isocyanate groups and a polyol having two or more active hydrogen groups. Can be used. Examples of the polyol include polyester polyol and / or polyether polyol. The said urethane resin may be used individually by 1 type, and may use 2 or more types together.

  Examples of the polyester polyol include ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, neopentyl glycol, 1,2-butylene glycol, 1,3-butylene glycol, 1 , 4-butylene glycol, 3-methylpentanediol, hexamethylene glycol, hydrogenated bisphenol A, trimethylolpropane, glycerin and other low molecular weight polyols, succinic acid, glutaric acid, adipic acid, sebacic acid, phthalic acid, isophthalic acid Polyesterification with hydroxyl groups at the ends obtained by reaction with polybasic acids such as acid, terephthalic acid, trimellitic acid, tetrahydrophthalic acid, endomethylenetetrahydrophthalic acid, hexahydrophthalic acid One or more objects and the like.

  Examples of the polyether polyol include ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, neopentyl glycol, 1,2-butylene glycol, 1,3-butylene glycol, Polyols such as 1,4-butylene glycol, 3-methylpentanediol, hexamethylene glycol, bisphenol A, hydrogenated bisphenol A, trimethylolpropane, and glycerin, or their ethylene oxide and / or propylene oxide high adducts, polyethylene glycol Polyether polyols such as polypropylene glycol and polyethylene / propylene glycol, polycaprolactone polyols, polyolefin polyols, One or more species of polybutadiene polyols to.

  Examples of the polyisocyanate include one or more of linear aliphatic, branched aliphatic, alicyclic and aromatic polyisocyanates. Specifically, for example, tetramethylene diisocyanate, hexamethylene diisocyanate, lysine diisocyanate ester, hydrogenated xylylene diisocyanate, 1,4-cyclohexylene diisocyanate, 4,4′-dicyclohexylmethane diisocyanate, 2,4′-dicyclohexylmethane diisocyanate. , Isophorone diisocyanate, 3,3′-dimethoxy-4,4′-biphenylene diisocyanate, 1,5-naphthalene diisocyanate, 1,5-tetrahydronaphthalene diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, 2,4'-diphenylmethane diisocyanate, phenylene diisocyanate, xylylene diisocyanate Sulfonates, and one or more such tetramethylxylylene diisocyanate.

  The polyester resin is a synthetic resin having an ester bond, and generally a resin obtained by a condensation reaction between a polybasic acid having two or more carboxyl groups and a polyol having two or more hydroxyl groups can be used. The said polyester resin may be used individually by 1 type, and may use 2 or more types together. Examples of the polybasic acid include succinic acid, glutaric acid, adipic acid, sebacic acid, phthalic acid, isophthalic acid, terephthalic acid, trimellitic acid, tetrahydrophthalic acid, endomethylenetetrahydrophthalic acid, and hexahydrophthalic acid. 1 type (s) or 2 or more types. On the other hand, examples of the polyol include polyester polyols and polyether polyols. More specifically, examples include the polyester polyols and polyether polyols described in detail in the section of the urethane resin.

  The vinyl acetate resin is a resin obtained by polymerization of vinyl acetate. The vinyl acetate resin also includes a resin in which less than 50% of vinyl acetate units in the polyvinyl acetate resin are hydrolyzed. The vinyl acetate resin is obtained not only by homopolymer of vinyl acetate but also by copolymerization of vinyl acetate and other monomers (for example, olefin such as ethylene), and the vinyl acetate unit is 50 mol% or more. Some copolymers are also included. The said vinyl acetate resin may be used individually by 1 type, and may use 2 or more types together.

  The polyvinyl alcohol resin is usually obtained by hydrolyzing polyvinyl acetate. As the polyvinyl alcohol resin, not only a completely hydrolyzed product but also a polyvinyl alcohol resin having a hydrolysis degree of 50% or more can be used. Furthermore, the polyvinyl alcohol resin includes an ethylene unit, and also includes a copolymer in which the ethylene unit is 50 mol% or less. The said polyvinyl alcohol resin may be used individually by 1 type, and may use 2 or more types together.

  The polyamide resin is a synthetic resin having an amide bond, and a resin obtained by a condensation reaction of a polybasic acid having two or more carboxyl groups and a polyamine having two or more amino groups can be used. Examples of the polybasic acid include succinic acid, glutaric acid, adipic acid, sebacic acid, phthalic acid, isophthalic acid, terephthalic acid, trimellitic acid, tetrahydrophthalic acid, endomethylenetetrahydrophthalic acid, hexahydrophthalic acid and the like. . On the other hand, polyamines include hydrazine, methylenediamine, ethylenediamine, propylenediamine, butylenediamine, hexanediamine, ethylaminoethylamine, methylaminopropylamine, iminobispropylamine, diethylenetriamine, triethylenetetramine, polyethyleneimine, diaminobenzene, triamino. Examples thereof include benzene, diaminoethylbenzene, triaminoethylbenzene, diaminoethylbenzene, triaminoethylbenzene, polyaminonaphthalene, polyaminoethylnaphthalene, and N-alkyl derivatives and N-acyl derivatives thereof. The said polyamide resin may be used individually by 1 type, and may use 2 or more types together.

  If the said fluorine-type resin is resin which contains a fluorine in a molecule | numerator, there will be no limitation in particular in the kind. Examples of the fluorine resin include (meth) acrylic resins containing fluorine in the molecule. The fluororesin may be a copolymer with other copolymerizable monomers. More specific examples of the fluororesin include, for example, polyvinylidene fluoride, ethylene-tetrafluoroethylene copolymer, trifluoromethyl polyacrylate, pentafluoroethyl polyacrylate, and fluoroalkyl (meth) acrylate (meth) acrylate. ) Alkyl acrylate copolymer. The said fluororesin may be used individually by 1 type, and may use 2 or more types together.

  In the lubricating film for plastic working of the present invention, as the resin constituting the resin layer, in addition to the resin composed of one or more of the above-mentioned resins, one or more of the above-mentioned resins And other resins may be used. As this composite resin, for example, a resin obtained by mixing one or more of the above-mentioned resins and other resin raw materials and various resins are grafted, blocked, etc. A composite resin having a structure derived from a plurality of monomers having different substituents can be used. In addition, a resin that is organically crosslinked or ionically crosslinked with a metal after film formation can be used.

  The content ratio of the resin having a glass transition temperature of 30 ° C. or less in the resin layer is 25 to 99 wt%, preferably 29.5 to 90 wt%, more preferably 30 to 30 wt% when the resin layer is 100 wt%. 80 wt%, more preferably 30 to 70 wt%, particularly preferably 30 to 60 wt%. When this content ratio is less than 25 wt%, the lubricating coating cannot sufficiently follow the expansion of the surface area of the workpiece during plastic processing. On the other hand, when the content ratio exceeds 99 wt%, no significant improvement in properties such as seizure resistance, moldability, and workability is observed, and it is difficult to recognize economic benefits.

  Further, the “wax particles” contained in the resin layer are melted by heat generated during processing as a lubricating coating component, and have an action of improving the slipping property of the coating. The structure and type of the wax particles are not particularly limited. As the wax particles, for example, natural wax and / or synthetic wax can be preferably used. More specifically, for example, one or two of paraffin wax, microcrystalline wax, petrolactam wax, (oxidized) polyethylene, (oxidized) polypropylene, carnauba wax, montan wax, candelilla wax, rice wax, lanolin and the like. The above can be mentioned. The wax particles in the present invention also include a polyethylene resin and a polypropylene resin.

  The physical properties of the wax particles are not particularly limited. For example, the average particle diameter of the wax particles can be in various ranges as required. The average particle size of the wax particles is usually 10 μm or less (for example, 0.001 to 10 μm), preferably 5 μm or less, more preferably 3 μm or less, more preferably 1 μm or less, and particularly preferably 0.001 to 1 μm. When the average particle diameter is in the above range, it is preferable because slipperiness can be imparted to the coating without reducing the strength of the coating. The wax particles preferably have a solid or viscosity at 100 ° C. of 10 mPa · s or more, preferably 20 mPa · s or more, more preferably 100 mPa · s or more. In this case, the plastic working of the metal in the cold state is preferable because it exhibits excellent lubricity even under severe processing conditions in which seizure is likely to occur.

  Further, the content ratio of the wax particles in the resin layer is preferably 0.5 to 74.5 wt%, more preferably 9.5 to 70 wt%, when the resin layer is 100 wt%. Preferably it is 19.5-69.5 wt%, More preferably, it is 29.5-69.5 wt%. When this content ratio is in the above range, it is preferable in cold plastic processing because it exhibits better lubricity even under severe processing conditions in which seizure is likely to occur.

  In the lubricating film for plastic working of the present invention, in order to further improve the lubricating effect during plastic working, an extreme pressure additive may be contained in the resin layer as necessary. The inclusion of such an extreme pressure additive is preferable because the lubrication performance in the extreme pressure lubrication region is improved and the seizure prevention effect becomes more remarkable.

  Examples of the extreme pressure additive include a sulfur-based extreme pressure additive, a phosphorus-based extreme pressure additive, and a chlorine-based extreme pressure additive. In addition, these may be used individually by 1 type and may use 2 or more types together. Examples of the sulfur-based extreme pressure additive include sulfurized olefins, sulfurized esters, thiocarbonates, dithiazoles, polythiazoles, thiols, thiocarboxylic acids, thiocols, sulfur, (poly) sodium sulfide, and the like. It is done. Examples of the phosphorus extreme pressure additive include condensed phosphates such as sodium tripolyphosphate and (sub) phosphate esters such as tricresyl phosphate. Furthermore, examples of the chlorinated extreme pressure additive include chlorinated paraffin, chlorinated fatty oil, polyvinylidene chloride, polyvinyl chloride, and vinylidene chloride-acrylic copolymer.

  The content ratio of the extreme pressure additive in the resin layer is preferably 0.5 to 74.5 wt% in terms of solid content, more preferably 1 to 70 wt% when the resin layer is 100 wt%. More preferably, it is 5 to 69.5 wt%. When the content ratio of the extreme pressure additive is within the above range, it is preferable because the lubrication performance in the extreme pressure lubrication region can be further improved and the seizure prevention effect can be further improved.

  Moreover, in the lubricating film for plastic working of the present invention, in order to improve the lubricating effect at the time of plastic working, the resin layer may contain fine particles as necessary. The inclusion of such fine particles is preferable because the shear strength and adhesion strength of the resin layer is increased, and the presence of the fine particles at the processing interface suppresses contact between metals and makes the seizure prevention effect more remarkable.

Examples of the fine particles include solid lubricants that can be expected to have an effect of reducing friction when they themselves have lubricity. Specific examples of such solid lubricants include molybdenum disulfide, tungsten disulfide, calcium stearate, mica, graphite, polytetrafluoroethylene (PTFE) and other lubricating resins, and complex oxides having an oxygen-defect perovskite structure ( Sr _x Ca _1-x CuO _y ) and the like. In addition, carbonates (such as carbonates of alkali metals or alkaline earth metals such as Na ₂ CO ₃ , CaCO ₃ , MgCO ₃ ), silicates (M _x O _y SiO ₂ [M: alkali metals, alkaline earth metals] ], Metal oxides (oxides of typical metal elements, oxides of transition metal elements, and complex oxides containing such metal elements [Al ₂ O ₃ / MgO, etc.]), sulfides (PbS, etc.) , Fluoride (CaF ₂ , BaF ₂ etc.), carbide (SiC, TiC), nitride (TiN, BN, AlN, Si ₃ N ₄ etc.), cluster diamond, and fullerene C ₆₀ or C ₆₀ and C ₇₀ Examples of such a mixture include fine particles that can suppress direct contact between metals without extremely reducing the friction coefficient and can be expected to have an anti-seizure effect. Examples of the oxide of the typical metal element include Al ₂ O ₃ , CaO, ZnO, SnO, SnO ₂ , CdO, PbO, Bi ₂ O ₃ , Li ₂ O, K ₂ O, Na ₂ O, and B ₂ O. ₃ , SiO ₂ , MgO, In ₂ O _{3 and the} like. Among these, the typical metal element is preferably an alkaline earth metal, aluminum, or zinc. Examples of the oxide of the transition metal element include TiO ₂ , NiO, Cr ₂ O ₃ , MnO ₂ , Mn ₃ O ₄ , ZrO ₂ , Fe ₂ O ₃ , Fe ₃ O ₄ , Y ₂ O ₃ , and CeO _2. , CuO, MoO ₃ , Nd ₂ O _3, and Ho ₂ O ₃ . Among these, those in which the transition metal element is iron or copper are preferable.
When the dissociation group contained in the resin in the resin layer is in a free form (for example, a free carboxyl group), avoid using fine particles (for example, a metal compound) reactive with the free group, Alternatively, in anticipation of dissolution of the fine particles due to the reaction with free radicals, the fine particles may be used in excess. Moreover, the said microparticles | fine-particles may be used individually by 1 type, and may use 2 or more types together.

  Further, the average particle diameter of the fine particles is not particularly limited, and can be set in various ranges as necessary. The average particle diameter of the fine particles is usually 10 μm or less (for example, 0.001 to 10 μm), preferably 5 μm or less, more preferably 2 μm or less. When the fine particles are flaky, the average particle size is the average value of the maximum particle sizes. In addition, some types of fine particles have a wide particle size distribution, but in the present invention, a desired effect can be obtained if 80% of the total fine particles are within the above range by volume. When the average particle size of the fine particles is 0.005 μm or more, it is preferable that the particles are prevented from aggregating in the resin, uniform dispersion is facilitated, and the removal treatment of the fine particles is facilitated after use. On the other hand, when the average particle size of the fine particles is 10 μm or less, the adhesion strength is improved, and as a result, the seizure prevention effect due to the contact between metals is improved.

The fine particles having the above average particle diameter are commercially available, and may be appropriately selected from commercially available products in consideration of dispersibility in the resin and / or wax used together. As an example of a commercial item (average particle size in parentheses), from “NanoTek” manufactured by CI Kasei, Al ₂ O ₃ (33 nm), TiO ₂ (30 nm), Fe ₂ O ₃ (21 nm), ZnO (31 nm), _{Y 2 O 3 (20nm),} CeO 2 (11nm), Mn 3 O 4 (38nm), SiO 2 (12nm) or the like, manufactured by Nippon Shokubai Co. of "SEAHOSTAR KE" P10 from (amorphous silica) (70 to 130 nm) , P50 (0.48 to 0.58 μm), P100 (0.9 to 1.1 μm), etc., “SEC Fine Powder SGP” (high purity artificial graphite 3 μm) manufactured by ESC, “AEROSIL” from SiO ₂ manufactured by Nippon Aerosil 50 "(30 nm)," AEROSIL 200 "(12 nm)," AEROSIL 300 "(7 nm)," C "from the _Al 2 _{O 3} (1 nm), 21nm "T805" and "P25" (both from TiO _2), etc., manufactured by Nissan Chemical Industries, Ltd. "SNOWTEX C" from SiO ₂ of and "Snowtex N" (both 20nm), etc., Ishihara Techno Co. of ultra-fine particles From Titanium oxide to “TTO-55 (B)” (30-50 nm), etc., from active calcium carbonate made by Kamishima Chemical Industries, “Culcise P” (0.10 μm), “Culcise PL10” (0.09 μm), “PLS2301” (40 nm), “EC” (1.0 to 2.0 μm) from light calcium carbonate, “Cluster Diamond” (5 nm) available from Tokyo Progress System, etc., “Lublon LDW-40” ( 0.18 μm), “L-2” (5 μm), etc. from “Teflon” (registered trademark) of Mitsui DuPont Fluorochemical LP-10F-1 "(2 [mu] m) or the like, Sumitomo Cement manufactured _{SiC (10nm), ZrO 2 (} 30nm), " molybdenum disulfide C powder produced by Osaka shipyard "(1.2 [mu] m), and the like.

  Further, when the fine particles are contained, the content ratio of the fine particles in the resin layer is not particularly limited, and can be appropriately adjusted as necessary. Specifically, when the resin layer is 100 wt%, it is preferably 0.01 to 10 wt%, more preferably 0.01 to 5 wt%, and still more preferably 0.05 to 1 wt%. It is preferable that the content ratio of the fine particles is within the above range because the shear strength and adhesion strength of the coating film formed when dried can be improved.

  Furthermore, in the lubricating film for plastic working of the present invention, the resin layer may be a general plastic working oil, in addition to the resin, wax particles, fine particles and extreme pressure additive, as long as the object of the present invention is not impaired. Additives that are added to can be added. Examples of such additives include pH adjusters, viscosity adjusters, preservatives, and antifoaming agents. Further, if necessary, a plasticizer, an oily agent, other extreme pressure additives, etc. may be used in combination. The resin layer may or may not contain a resin having a glass transition temperature exceeding 30 ° C. as another resin. Here, “not contained” includes not only a case where it is not contained at all, but also a case where a trace amount of a resin having a glass transition temperature exceeding 30 ° C. is contained within a range not impairing the object of the present invention. .

  The “base material” on which the lubricating film for plastic working of the present invention is formed may be a raw material for plastic working or a metal mold used for plastic working. That is, the lubricating film for plastic working of the present invention can be formed on the surface of a material to be subjected to plastic working and / or on the molding surface of a metal mold used for plastic working. There is no particular limitation on the material of the base material in the lubricating film for plastic working of the present invention. The material of the base material is usually mainly steel, such as iron, carbon steel, and stainless steel, and an iron alloy. In addition, "Inconel" (trade name), titanium, titanium alloy, aluminum, aluminum alloy, magnesium, magnesium Non-ferrous metals such as alloys, copper, and copper alloys may also be used. Also, the shape of the base material is not particularly limited because it is possible to process not only raw materials such as rods and block materials but also shapes (such as gears and shafts) after hot forging.

  Prior to forming the lubricating film for plastic working of the present invention on the base material, the base material can be subjected to pretreatment such as degreasing with an alkaline degreasing agent, washing with water, pickling with hydrochloric acid or the like. By performing such pretreatment, the surface of the base material can be kept clean. As a result, the adhesion between the base material and the lubricating coating is improved, and scratches after processing due to contamination such as earth and sand are generated. It is preferable because good results such as prevention can be obtained. In addition, when the lubricating film for plastic working of the present invention is formed using the composition for forming a lubricating film for plastic working of the present invention described later, the composition for forming a lubricating film for plastic working of the present invention is uniform on the surface of the base material. It is preferable because the adhesion between the base material and the lubricating coating can be improved. Usually, pretreatment is performed in the order of degreasing, water washing, pickling and water washing, but the order is not particularly limited. For example, in the case of a base material to which no oxide scale is attached, the pickling and rinsing steps may be omitted. The pretreatment may be performed by a conventional method and is not particularly limited.

  Furthermore, in order to increase the adhesion between the lubricating film for plastic working of the present invention and the base material, it is effective to increase the surface roughness of the base material. Although the above-mentioned pickling is effective, there are other mechanical methods such as grinding with rough abrasive paper or a metal brush, shot blasting, shot peening, and the like. Furthermore, phosphoric acid-based chemical conversion treatment with manganese phosphate or zinc phosphate, oxalate-based chemical conversion treatment, or the like is also effective.

  The lubricating film for plastic working of the present invention may be formed on the entire base material, but may be formed only on a specific portion. For example, plastic working that requires lubricity at a specific location on the contact surface between the tool for plastic working and the workpiece, for example, seizure of roll-passing edge portions in plate rolling, and perforated roll in tube rolling When the objective is to prevent seizure at the tube outer shape contact portion, the lubricating film for plastic working of the present invention may be formed only at that portion.

  The lubricating coating for plastic working of the present invention is used for various metal working, especially cold rolling of metal such as plate rolling, pipe rolling, strip steel (section steel, bar wire, wire rod) rolling, drawing (drawing), forging, etc. It can be suitably used. Especially, it is particularly effective for steel pipe drawing. This is because the lubricating film for plastic working of the present invention effectively acts and can prevent seizure even in severe processing and friction generated at the contact surface between the inner surface of the tube and the plug in drawing of the steel tube. This point will be described in more detail. First, the pipe before drawing is not necessarily along the tool (die, plug), but the pipe is deformed so as to follow the tool at the start of drawing. At this time, a part having a high surface pressure is locally generated, but there are particularly many places where such a part is generated on the inner surface of the tube and the plug surface, and the surface pressure at that time is also high. At the stage immediately after the start of drawing, the surface temperature of the tube and plug is still around room temperature, and the resin whose glass transition temperature is not adjusted cannot follow the friction surface on which the coating film is deformed and is detached, and is burned on the inner surface of the tube. May cause sticking. Even in the case of an oil type lubricant, the same type of seizure is likely to occur because reactive additives do not work in this temperature range. However, the lubricating film for plastic working of the present invention does not cause seizure because the film is optimized at the glass transition temperature so that the film can follow the change of the friction surface even in these temperature ranges.

  In addition, the lubricating film for plastic working of the present invention is not subjected to plastic working, and is merely used as a rust preventive film treatment at the time of product shipment, or a surface for preventing wrinkles due to contact with rollers and guides during work material transportation. It can also be used for protection and friction reduction applications. In any case, when the coating is no longer necessary after plastic processing or without plastic processing, the plastic processing resin coating of the present invention can be easily removed with a solvent or a cleaning agent.

(2) Lubricating film forming composition for plastic working The composition for forming a lubricating coating for plastic working of the present invention contains a resin having a glass transition temperature of 30 ° C. or lower and wax particles in a solvent. As described above, in the conventional chemical conversion film treatment, a lubricant is applied onto the formed chemical conversion film, and therefore, including water washing and pickling, many treatment steps are required (FIG. 1A). On the other hand, if a film is formed using the composition for forming a lubricating film for plastic working of the present invention, as shown in FIG. 1 (B), the chemical conversion treatment and the accompanying pickling and water washing are omitted. Can do. As a result, a lubricating film can be easily formed, and when this lubricating film forming composition for plastic working is used, it is possible to prevent environmental pollution caused by waste generated by the conventional chemical conversion film treatment. It is also possible to omit the provision of such a waste disposal facility.

  Examples of the “solvent” include water, alcohols, ether solvents, acetate solvents, ketone solvents, hydroxyamines, dimethyl sulfoxide and the like. These can be used individually by 1 type or in combination of 2 or more types. The solvent is considered to be involved in the formation of a tough resin layer. It is preferable to use water or a solvent containing at least water as the solvent because a tough film can be more reliably formed. Examples of the solvent containing at least water include a mixed solvent composed of water and a solvent other than water. More specifically, for example, a water-alcohol solvent composed of water and the above alcohols can be used.

  Examples of the alcohols include methanol, ethanol, 1-propanol, 2-propanol, n-butanol, 2-butanol, t-butanol, 2-ethylbutanol, 2-ethylhexanol, and 3-methyl-3-methoxybutanol. Benzyl alcohol, phenol, ethylene glycol, propylene glycol, 1,3-butyldiol, 2-ethyl-1,3-hexanediol, 3-methyl-1,3-butanediol, and glycerin.

  Examples of the ether solvents include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol diethyl ether, ethylene glycol monopropyl ether, ethylene glycol monoalkyl ethers such as ethylene glycol monobutyl ether, ethylene glycol dialkyl ethers, Diethylene glycol monoalkyl ethers such as diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol diethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, diethylene glycol dialkyl ethers, polyethylene glycol monoalkyl ethers, polyethylene glycol dialkyl Ethers, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol diethyl ether, propylene glycol monopropyl ether, propylene glycol monoalkyl ethers such as propylene glycol monobutyl ether, propylene glycol dialkyl ethers, dipropylene glycol monomethyl ether, Dipropylene glycol monoalkyl ethers such as dipropylene glycol monoethyl ether, dipropylene glycol diethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, dipropylene glycol dialkyl ethers, polypropylene glycol monoalkyl ethers, polypropylene glycol Dialkyl ethers, 1,4-dioxane, tetrahydrofuran and the like.

  Examples of the acetate solvent include the above-described alcohols or acetylated products of ether solvents having a hydroxyl group.

  Examples of the ketone solvent include acetone, methyl ethyl ketone, methyl isobutyl ketone, 2-pyrrolidone, N-methyl-2-pyrrolidone, N-methyl-3methyl-2-pyrrolidone, 1,3-dimethyl-2-imidazolide. Non, N, N-dimethylformamide and the like can be mentioned.

  Examples of the hydroxyamines include monoethanolamine, N-ethylethanolamine, Nn-butylethanolamine, N, N-dimethylethanolamine, N, N-diethylethanolamine, N, N-dibutylethanolamine. , Diethanolamine, N-ethyldiethanolamine, Nn-butyldiethanolamine, triethanolamine, isopropanolamine, N- (β-aminoethyl) isopropanolamine, N, N-diethylisopropanolamine and the like.

Regarding the above-mentioned “resin having a glass transition temperature of 30 ° C. or lower”, the above description is valid as it is. The glass transition temperature is 30 ° C. or lower, preferably 26 ° C. or lower, more preferably 23 ° C. or lower, more preferably 15 ° C. or lower, and particularly preferably 10 ° C. or lower. In addition, about the minimum of the range of the said glass transition temperature, it can set suitably, -85 degreeC is mentioned as an example.
The resin having a glass transition temperature of 30 ° C. or lower is at least one of (meth) acrylic resin, urethane resin, polyester resin, vinyl acetate resin, polyvinyl alcohol resin, polyamide resin, and fluorine resin. More preferred. The resin may be an uncrosslinked polymer or a crosslinked polymer. The cross-linked polymer is preferably a resin cross-linked with a compound containing at least one metal element of the above-described typical metal element and transition metal element and / or ions thereof. In particular, the aforementioned ionomer is preferable. When an uncrosslinked polymer is used, a film is formed by further adding a crosslinking agent such as an organic crosslinking agent or an ionic crosslinking agent such as a compound containing a metal element to the lubricating film forming composition for plastic working. It can also be crosslinked later.
Further, the content ratio of the resin having a glass transition temperature of 30 ° C. or less is 25 to 99 wt%, preferably 30 to 30 wt% when the solid content of the lubricating film forming composition for plastic working of the present invention is 100 wt%. 90 wt%, more preferably 30 to 80 wt%, more preferably 30 to 70 wt%, particularly preferably 30 to 60 wt%.

  Moreover, the form at the time of suspending or disperse | distributing the resin whose said glass transition temperature is 30 degrees C or less in the said solvent is not specifically limited. For example, it may be a resin melt having a glass transition temperature of 30 ° C. or lower, or water, an organic solvent (alcohol, mineral oil, mineral spirit, methyl ethyl ketone, “Freon” (trade name), etc.), or water and an organic solvent. And a solution or dispersion dissolved or dispersed in a mixed solvent. Moreover, the form which mixes at the time of use by preparing 2 or more types of containing liquids containing a part of resin which forms the said resin layer may be sufficient.

  Furthermore, when the resin having a glass transition temperature of 30 ° C. or lower is suspended or dispersed in a solvent, a plasticizer may be used as necessary. By using such a plasticizer, the resin having a glass transition temperature of 30 ° C. or lower can be uniformly suspended or dispersed. Furthermore, the glass transition temperature of a resin having a glass transition temperature of 30 ° C. or lower can be lowered. The said plasticizer is not specifically limited, The compound generally used as a plasticizer for resin can be used. Specific examples include phthalic acid esters, adipic acid esters, sebacic acid esters, trialkyl trimellitic acid, (phosphite) phosphoric acid esters, chlorinated paraffins, and the like. These may be used alone or in combination of two or more.

  With respect to the “wax particles”, the above description is valid as it is. That is, the above-mentioned particles can be used as the types of the wax particles. The average particle size of the wax particles is preferably 10 μm or less, more preferably 10 μm or less (for example, 0.001 to 10 μm), more preferably 5 μm or less, and particularly preferably 3 μm or less. Furthermore, the wax particles preferably have a solid or viscosity at 100 ° C. of 10 mPa · s or more, preferably 20 mPa · s or more, more preferably 100 mPa · s or more.

  The content ratio of the wax particles is preferably 0.5 to 74.5 wt%, more preferably 9.5 to 0.5 wt% when the solid content of the lubricating film forming composition for plastic working is 100 wt%. It is 70 wt%, more preferably 19.5-69.5 wt%, more preferably 29.5-69.5 wt%. When this content ratio is in the above range, it is preferable in cold plastic processing because it exhibits better lubricity even under severe processing conditions in which seizure is likely to occur.

  The form when the wax particles are suspended or dispersed in a solvent is not particularly limited. For example, a water dispersion or water emulsion of wax particles may be contained in the solvent, or the wax particles may be contained as they are.

  In the composition for forming a lubricating film for plastic working of the present invention, when the resin having the glass transition temperature of 30 ° C. or lower and the wax particles are suspended or dispersed in a solvent, a surfactant may be used as necessary. it can. By using such a surfactant, the resin and the wax particles can be uniformly suspended or dispersed. Further, the resin layer formed on the surface of the base material has good lubricity and can effectively prevent the material and the mold from being seized.

  As the surfactant, any of a nonionic surfactant, an anionic surfactant, an amphoteric surfactant and a cationic surfactant can be used. Examples of the nonionic surfactant include polyoxyethylene alkyl ether, polyoxyalkylene (ethylene and / or propylene) alkyl phenyl ether, polyethylene glycol (or ethylene oxide) and higher fatty acids (for example, straight chain having 12 to 18 carbon atoms). And polyoxyethylene sorbitan alkyl esters composed of sorbitan, polyethylene glycol and higher fatty acids (for example, linear or branched fatty acids having 12 to 18 carbon atoms). Etc. Examples of the anionic surfactant include fatty acid salt, sulfate ester salt, sulfonate salt, phosphate ester salt, and dithiophosphate ester salt. Examples of amphoteric surfactants include amino acid type and betaine type carboxylates, sulfate esters, sulfonates, and phosphate ester salts. Examples of the cationic surfactant include aliphatic amine salts and quaternary ammonium salts. The said surfactant may be used individually by 1 type, and may be used in combination of 2 or more type.

  In addition, the composition for forming a lubricating coating for plastic working of the present invention may contain an extreme pressure additive as necessary in order to further improve the lubricating effect during plastic working. The above description is valid for the extreme pressure additive. That is, as the extreme pressure additive, for example, at least one of the aforementioned extreme pressure additives can be used. The content of the extreme pressure additive is preferably 0.5 to 74.5 wt% in terms of solid content when the solid content of the lubricating film forming composition for plastic working is 100 wt%, More preferably, it is 1-70 wt%, More preferably, it is 5-69.5 wt%.

  Furthermore, the composition for forming a lubricating coating for plastic working of the present invention may contain fine particles as necessary in order to further improve the lubricating effect during plastic working. The above description is valid for the fine particles. That is, as the fine particles, one or more of the fine particles described above can be used. Moreover, the content rate of the said microparticles | fine-particles is not specifically limited, It can adjust suitably as needed. Specifically, when the solid content of the lubricating film forming composition for plastic working is 100 wt%, it is preferably 0.01 to 10 wt%, more preferably 0.01 to 5 wt%, still more preferably May be 0.05 to 1 wt%.

  Further, when the fine particles are contained, the content ratio of the fine particles in the resin layer is not particularly limited, and can be appropriately adjusted as necessary. Specifically, when the resin layer is 100 wt%, it is preferably 0.01 to 10 wt%, more preferably 0.01 to 5 wt%, and still more preferably 0.05 to 1 wt%. It is preferable that the content ratio of the fine particles is within the above range because the shear strength and adhesion strength of the coating film formed when dried can be improved.

  The method for mixing the fine particles is not particularly limited as long as a composition in which the fine particles are uniformly dispersed is obtained. For example, if the fine particles are fine particles that are not reactive with the reaction components used for the synthesis of the resin, the fine particles may be included during the synthesis of the resin. Moreover, it can carry out by the method of mixing solid microparticles | fine-particles simultaneously with resin and wax particle | grains melt | dissolved or disperse | distributed to the solvent.

  The composition for forming a lubricating film for plastic working of the present invention is not limited to the solvent, resin, wax particles, fine particles, extreme pressure additive, surfactant, and plasticizer, as long as the object of the present invention is not impaired. Moreover, the additive currently added to the general plastic processing oil agent can be added. Examples of such additives include pH adjusters, viscosity adjusters, preservatives, crosslinking agents, and antifoaming agents. Further, other extreme pressure additives, oily agents and the like may be used in combination as necessary. Furthermore, the resin for forming a lubricating film for plastic working may or may not contain a resin having a glass transition temperature exceeding 30 ° C. Here, “not contained” includes a trace amount of a resin having a glass transition temperature exceeding 30 ° C. in the range not impairing the purpose of the present invention as well as the case where it is not contained at all. This includes cases where

(3) Material for plastic working The material for plastic working of the present invention is characterized in that the lubricating film for plastic working of the present invention is formed on the surface of a material for producing a plastic processed product having an arbitrary shape. And This plastic working material exhibits good seizure resistance, formability, and workability in any secondary processing at a processing manufacturer, and can protect the plastic working material from contact flaws during conveyance.

The material of the material is not particularly limited, and the description of the material of the base material is valid as it is. In addition, as described in the above-mentioned base material, the lubricating film for plastic working of the present invention is also formed on the above-mentioned raw material in order to improve the adhesion between the raw material and the lubricating film for plastic working of the present invention. Prior to pre-treatment such as degreasing, washing with water, pickling, etc., or
The surface roughness of the material can be increased.

  In the material for plastic working of the present invention, the method for forming the lubricating film for plastic working of the present invention on the surface of the material is not particularly limited. For example, by applying a liquid material such as a solution containing a component constituting the lubricating film for plastic working of the present invention to the material and drying it, like the above-described composition for forming a lubricating film for plastic working of the present invention. Can be formed.

  There is no particular limitation on the coating method, and various methods can be used as necessary. For example, when applying on the surface of a raw material, arbitrary methods, such as immersing a raw material in the said liquid substance, apply | coating with a brush, spray application, or pouring, are employable. Moreover, when apply | coating to the shaping | molding surface of a type | mold, methods, such as apply | coating with a brush, spray application, and pouring, can be employ | adopted. Application of the liquid material is not particularly limited as long as the surface of the base material is sufficiently covered with the lubricating film for plastic working.

  The drying method is not particularly limited as long as the lubricating film for plastic working of the present invention can be formed. For example, the material or mold coated with the liquid material may be left to dry naturally, or may be forced to dry as necessary. In the case of forced drying, an arbitrary method such as a method of irradiating ultraviolet rays, a method of applying hot air, a method of preheating a material or a mold, a method of drying by high-frequency heating can be adopted. Such forced drying is preferably performed at 60 to 150 ° C. for about 10 to 60 minutes.

  In the material for plastic working according to the present invention, the lubricating film for plastic working according to the present invention may be formed on the entire material, but may be formed only on a specific portion. For example, plastic working that requires lubricity at a specific location on the contact surface between the tool for plastic working and the workpiece, for example, seizure of roll-passing edge portions in plate rolling, and perforated roll in tube rolling When the objective is to prevent seizure at the tube outer shape contact portion, the lubricating film for plastic working of the present invention may be formed only at that portion.

In the plastic working material of the present invention, the weight, thickness, etc. of the lubricating film for plastic working of the present invention are not particularly limited, and can be in various ranges as required. For example, the weight of the resin layer constituting the lubricating film for plastic working of the present invention or the lubricating film for plastic working of the present invention is preferably 1 g / m ² or more from the viewpoint of preventing seizure, and 30 g from the viewpoint of cost. / M ² or less is preferable. More preferably, it is 3-20 g / m < ² >, More preferably, it is 5-15 g / m < ² >. Further, the thickness of the lubricating film for plastic working of the present invention is usually a uniform thickness, but lubricity is particularly required at a specific portion of the contact surface between the plastic working tool and the workpiece. In a plastic working material used for plastic working, only a specific part can be thickened.

(4) Manufacturing method of plastic processed product and manufacturing method of metal tube, metal wire or metal rod The manufacturing method of the plastic processed product of the present invention is characterized by plastic processing the material for plastic processing of the present invention. Moreover, the manufacturing method of the metal tube of this invention, a metal wire, or a metal bar is characterized by drawing the raw material for plastic working of this invention.

  Examples of the plastic working include cold plastic working of metals such as plate rolling, pipe rolling, strip steel (section steel, bar wire, wire rod) rolling, drawing (drawing), and forging. There are no particular limitations on the conditions and methods for plastic working, and there are no particular limitations on the conditions and methods for forming the lubricating film for plastic working. For example, in cold drawing, the drawing wire is usually immersed in a tank containing the composition for forming a lubricating film for plastic working of the present invention, or the lubricating film for plastic working is formed using a nozzle. The composition is applied by a general application method such as spraying the drawing wire. Next, after passing through a dry zone of 60 to 150 ° C. as necessary to form a lubricating film for plastic working having a desired thickness, the film is drawn by a die. Alternatively, the coating can be formed by batch processing. That is, after the wire wound in a coil shape is immersed in a tank containing the composition for forming a lubricating film for plastic working according to the present invention, it is placed in a drying furnace at 60 to 150 ° C. to form a film, and unwinding Draw. Moreover, after immersing in a tank, you may unwind a coil and let the above-mentioned 60-150 degreeC dry zone pass, and may form a film. On the other hand, in cold drawing of steel pipes, the coating on the outer surface may be formed in the same manner as the wire, but the inner surface is immersed in a tank containing the lubricating film forming composition for plastic working of the present invention, or a nozzle Is applied to the inner surface of the tube and sprayed or the like, and then the solution is applied, and then a film is formed by placing in a drying furnace at 60 to 150 ° C. or passing through a drying zone. The film remaining on the surface of the wire and the steel pipe is completely removed with a subsequent solvent or cleaning agent.

  Also, in hydroforming (hydraulic bulge forming), after forming the lubricating film for plastic working of the present invention on the outer surface of the raw tube, which is a work material, molding is performed to reduce friction, the work material and the mold surface. Anti-wrinkle can be achieved. In addition, since the resin film is removed with a solvent or a cleaning agent after processing, it is advantageous in terms of equipment and running cost as compared with a chemical film treatment such as a zinc phosphate treatment.

  Hereinafter, the present invention will be described specifically by way of examples. In addition, this invention is not limited to a following example. In the description of this example, “part” is based on mass and “%” indicates “wt%”.

[1] Preparation of composition for forming lubricating film for plastic working (1) Raw materials used (a) Resin component 1: 50 parts of water and 0.1 part of sodium lauryl sulfate were charged into a separable flask equipped with a stirrer, a thermometer and a reflux condenser, and the temperature was raised to 80 ° C. while stirring and replacing with nitrogen. Thereafter, the internal temperature was kept at 80 ° C., and 0.1 part of potassium persulfate was added as a polymerization initiator. After dissolution, 0.3 part of methyl methacrylate, 0.6 part of butyl acrylate, 0.05 part of acrylic acid , 0.05 part of methacrylic acid and 0.01 part of lauryl mercaptan were charged and reacted for 1 hour. Then, after completion of the reaction, under stirring 150 parts of water, 0.5 part of sodium lauryl sulfate, 1 part of lauryl mercaptan, 30 parts of methyl methacrylate, 60 parts of butyl acrylate, 5 parts of acrylic acid and 5 parts of methacrylic acid. In addition to the mixed solution B prepared in addition to the above, an aqueous solution in which 1 part of potassium persulfate was dissolved in 20 parts of water was continuously added over 4 hours to cause the reaction. After completion of the addition, the mixture was further aged for 4 hours. The emulsion was cooled to room temperature, adjusted to pH 8.5, solid content of 25% with 10% potassium hydroxide aqueous solution and water, and resin solution no. 1 was prepared.

No. 2; In place of the mixed solution B used for the preparation of the resin solution 1, water 150 parts, sodium lauryl sulfate 0.5 part, lauryl mercaptan 1 part, methyl methacrylate 15 parts, styrene 15 parts, butyl acrylate 60 parts, Except for using a mixed solution prepared by adding 5 parts of acrylic acid and 5 parts of methacrylic acid under stirring, the above resin No. 1 was used. What was prepared by the method similar to 1 was used.
No. 3; In place of the mixed solution B used for the preparation of the resin solution 1, water 150 parts, sodium lauryl sulfate 0.5 part, lauryl mercaptan 1 part, methyl methacrylate 40 parts, butyl acrylate 50 parts, acrylic acid 5 parts And 5 parts of methacrylic acid was added with stirring, except that the mixed solution prepared above was used. What was prepared by the method similar to 1 was used.

  No. 4: In a separable flask equipped with a stirrer, a thermometer and a reflux condenser, 390 parts of 2-propanol, 40 parts of methyl methacrylate, 50 parts of butyl acrylate, 5 parts of acrylic acid, 5 parts of methacrylic acid, 1 part of lauryl mercaptan, Then, 0.5 parts of azobisisobutyronitrile was added, the atmosphere was replaced with nitrogen while stirring, and the mixture was reacted for 8 hours under reflux. After cooling to room temperature, it was adjusted with 2-propanol so that the solid content was 20%. 4 was prepared.

No. 5; In place of the mixed solution B used for the preparation of the resin solution 1, water 150, water lauryl sulfate 0.5 part, lauryl mercaptan 1 part, methyl methacrylate 45 parts, butyl acrylate 45 parts, acrylic acid 5 parts And 5 parts of methacrylic acid was added with stirring, except that the mixed solution prepared above was used. What was prepared by the method similar to 1 was used.
No. 6; In place of the mixed solution B used for the preparation of the resin solution No. 1, water 150 parts, sodium lauryl sulfate 0.5 part, lauryl mercaptan 1 part, methyl methacrylate 50 parts, butyl acrylate 40 parts, acrylic acid 5 parts And 5 parts of methacrylic acid was added with stirring, except that the mixed solution prepared above was used. What was prepared by the method similar to 1 was used.
No. 7; In place of the mixed solution B used for the preparation of the resin solution 1, water 150 parts, sodium lauryl sulfate 0.5 parts, lauryl mercaptan 1 part, methyl methacrylate 55 parts, butyl acrylate 35 parts, acrylic acid 5 parts And 5 parts of methacrylic acid was added with stirring, except that the mixed solution prepared above was used. What was prepared by the method similar to 1 was used.

  No. 8; A separable flask equipped with a stirrer, a thermometer, and a reflux condenser was charged with 250 parts of water, 0.2 part of sodium lauryl sulfate, and 0.5 part of polyoxyethylene alkyl ether. The temperature was raised to ° C. Thereafter, the internal temperature was kept at 80 ° C., and 0.1 part of potassium persulfate was added as a polymerization initiator. After dissolution, 0.6 parts of methyl methacrylate, 0.35 part of butyl acrylate, 0.05 part of methacrylic acid And a mixed solution of 0.01 part of lauryl mercaptan were charged and reacted for 1 hour. Then, after completion of the reaction, a mixed solution of 60 parts of methyl methacrylate, 35 parts of butyl acrylate, 5 parts of methacrylic acid, and 1 part of lauryl mercaptan, and an aqueous solution in which 1 part of potassium persulfate was dissolved in 20 parts of water, It was continuously added over 4 hours and allowed to react. After completion of the addition, the mixture was further aged for 4 hours, and the emulsion was cooled to room temperature, adjusted with 8% aqueous ammonia and water to a pH of 8.5 and a solid content of 25%. 8 was prepared.

No. 9; In place of the mixed solution B used for the preparation of the resin solution 1, water 150, water lauryl sulfate 0.5 part, lauryl mercaptan 1 part, methyl methacrylate 60 parts, butyl acrylate 30 parts, acrylic acid 5 parts And 5 parts of methacrylic acid was added with stirring, except that the mixed solution prepared above was used. What was prepared by the method similar to 1 was used.
No. 10; 9 (resin content: 25%) prepared by adding 2.5 parts of tri (2-butoxyethyl) phosphate and 7.5 parts of water to 100 parts of resin No. 9 and stirring for a whole day and night was used.

No. 11; Daiichi Kogyo Seiyaku Co., Ltd., water-based urethane resin (solid content: 32%)
No. 12: Daiichi Kogyo Seiyaku Co., Ltd. water-based urethane resin (solid content: 30%)
No. 13; manufactured by Toyobo Co., Ltd., water-based polyester resin (solid content: 15%)
No. 14; manufactured by Sumitomo Chemical Co., Ltd., ethylene-vinyl acetate (1: 1) copolymer suspension (solid content: 50%)
No. 15; Resin that completely saponified 14 (solid content: 100%)
No. 16; manufactured by BASF, polyvinylpyrrolidone aqueous solution (solid content: 20%)
No. 17; manufactured by Sumitomo Seika Co., Ltd., polyamide resin suspension (solid content: 40%)
No. 18; manufactured by Kanebo Corporation, phenol resin (solid content: 100%)
No. 19; Epoxy resin powder (solid content: 100%)
No. 20; manufactured by Sumitomo 3M Co., Ltd., polyfluorinated ethylene resin suspension (solid content: 53%)

No. 21: A separable flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 250 parts of water, 0.5 part of sodium lauryl sulfate, and 0.5 part of polyoxyethylene alkyl ether, and the mixture was purged with nitrogen while stirring. The temperature was raised to ° C. Thereafter, the internal temperature was kept at 80 ° C., and 0.1 part of potassium persulfate was added as a polymerization initiator. After dissolution, 0.45 part of methyl methacrylate, 0.5 part of butyl acrylate, 0.05 part of methacrylic acid And a mixed solution of 0.01 part of lauryl mercaptan were charged and reacted for 1 hour. Then, after completion of the reaction, a mixed solution of 45 parts of methyl methacrylate, 50 parts of butyl acrylate, 5 parts of methacrylic acid, and 1 part of lauryl mercaptan, and an aqueous solution in which 1 part of potassium persulfate was dissolved in 20 parts of water, It was continuously added over 4 hours and allowed to react. After completion of the addition, aging was further performed for 4 hours, and the emulsion was cooled to room temperature. Thereafter, 68.2 parts of a zinc crosslinking agent was added dropwise over 30 minutes. Next, the mixture was heated at 85 ° C. for 6 hours to allow the crosslinking reaction to proceed, then cooled to room temperature, adjusted with water to a solid content of 20%, 21 was prepared. The zinc crosslinking agent comprises 7 parts of zinc oxide, 12 parts of ammonium carbonate, 14 parts of 25% aqueous ammonia and 67 parts of water.
No. 22; Resin No. 21 except that 86.9 parts of a calcium crosslinking agent was used instead of the zinc crosslinking agent used in the preparation of the resin solution of No. 21. What was prepared by the method similar to 21 was used. In addition, the said calcium crosslinking agent is a dispersion liquid which consists of 5 parts of calcium oxide well ground in a mortar and 95 parts of water.

No. 1-No. The glass transition temperature of the resin component in the 22 resin solution is as follows. No. The glass transition temperatures of 1 to 10, 14, 15, 21, and 22 are values calculated from the FOX equation. In 21 and 22, it is the glass transition temperature of the resin before crosslinking. No. The glass transition temperatures of 11 to 13 and 16 are as described in the product brochure. Furthermore, no. The glass transition temperature of 17-20 was measured based on JIS K7121.

(B) Wax component No. 1: 75 parts of water, 20 parts of polyethylene oxide (softening point: 138 ° C., form at 100 ° C .: solid), 5 parts of polyoxyethylene alkyl ether and 0.2 part of potassium hydroxide are added to a high-pressure vessel, and 160 ° C. After stirring for 3 hours, the mixture was cooled to room temperature to prepare an emulsified wax solution (solid content: 25%).
No. 2: “Chemical Pearl W310” manufactured by Mitsui Chemicals, Inc. (solid content: 30%, softening point: 132 ° C.)
No. 3; 75 parts of water, 20 parts of polyethylene oxide (softening point: 106 ° C., form at 100 ° C .: solid), 5 parts of polyoxyethylene alkyl ether and 0.2 part of potassium hydroxide are added to a high-pressure vessel, and 160 ° C. After stirring for 3 hours, the mixture was cooled to room temperature to prepare an emulsified wax solution (solid content: 25%).
No. 4: 5 parts of polyoxyethylene alkyl ether was added to 20 parts of paraffin wax (softening point: 40 ° C., viscosity at 100 ° C .: 1 mPa · s), dissolved under stirring at 98 ° C., and then water 75 at 60 ° C. Portions were slowly added to prepare an emulsified wax solution (solid content: 25%).

No. 5; 75 parts of water, 20 parts of mixed wax, 5 parts of polyoxyethylene alkyl ether and 0.2 part of potassium hydroxide are added to a high pressure vessel, stirred at 160 ° C. for 3 hours, cooled to room temperature, and emulsified wax. A solution (solid content: 25%) was prepared. The mixed wax is a mixture of polyethylene oxide (softening point: 138 ° C.) and paraffin wax (softening point: 40 ° C.), and the viscosity at 100 ° C. adjusted to 20 mPa · s.
No. 6: Carnauba wax (viscosity at 100 ° C .: 22 parts mPa · s), 5 parts of polyoxyethylene alkyl ether were added and dissolved under stirring at 98 ° C., and then 75 parts of normal temperature water was slowly added to emulsify. A prepared wax solution (solid content: 25%) was prepared.
No. 7: To 20 parts of lanolin (viscosity at 100 ° C .: 27 mPa · s), 5 parts of polyoxyethylene alkyl ether was added and dissolved under stirring at 98 ° C., and then 75 parts of room temperature water was slowly added to emulsify. A wax solution (solid content: 25%) was prepared.
No. 8: 10 parts of carnauba wax (viscosity at 100 ° C .: 22 mPa · s) was added to 40 parts of 2-propanol, and a solution obtained by heating and dissolving at 80 ° C. was added to 50 parts of normal temperature 2-propanol stirred with a homomixer. Slowly added to prepare a wax solution (solid content: 10%).

No. 1-No. The average particle size of the wax particles in the wax component No. 8 is as follows.

(C) Solvent No. 1; Water No. 1 2; 2-propanol (IPA)
No. 3; N-methyl-2-pyrrolidone (NMP)
No. 4; diethylene glycol monoethyl ether 5; 2-ethanolamine 6; Acetone

(D) Extreme pressure additive No. 1; Phosphorus extreme pressure additive, sodium tripolyphosphate (anhydride)
No. 2: Phosphorus extreme pressure additive, tricresyl phosphate No. 2 3; Phosphorus extreme pressure additive, amine salt of dialkyl phosphate ester (manufactured by Sanyo Chemical Industries)
No. 4; Sulfur-based extreme pressure additive, dialkyl polysulfide (Dainippon Ink Chemical Co., Ltd.)
No. 5; sulfur-based extreme pressure additive, 2,2-dibenzothiazyl disulfide No. 5 6: Sulfur-based extreme pressure additive, dialkyldithiothiadiazole (Dainippon Ink Chemical Co., Ltd.)
No. 7: Chlorine extreme pressure additive, chlorinated paraffin (manufactured by Ajinomoto Co., Inc.)
No. 8: Chlorine extreme pressure additive, manufactured by BF-Goodrich, aqueous vinylidene chloride-acrylic copolymer (solid content: 58%)

(E) Fine particles 1; Fumed silica, manufactured by AEROSIL No. 1 2; scaly graphite 3; Zinc oxide, manufactured by Hakusuitec Co., Ltd. 4: Calcium oxide (calculated from Wako Pure Chemical Industries, Ltd., finely divided by a ball mill)

(2) Preparation of Lubricating Film Forming Composition for Plastic Processing Each raw material of the above (1) is mixed so as to have the combinations and blending amounts shown in Tables 3 to 6, and Examples 1 to 49 and Comparative Example 1 are mixed. A composition for forming a lubricating film for plastic working of ~ 4 was obtained. In Comparative Example 5, a non-water type lubricating oil (main component: fatty acid ester 15 wt%, sulfurized fat and oil 70 wt%) was used.

[2] Performance Evaluation of Examples Performance evaluation of each composition for forming a lubricating film for plastic working in Examples 1 to 49 and Comparative Examples 1 to 5 was performed by the following method.

(1) Cold drawing of steel pipe by a small drawing machine A steel pipe (SUS304) having an outer diameter of 25.4 mm, an inner diameter of 21.4 mm, and a length of 800 mm was used as a workpiece. The steel pipe is subjected to a solution treatment in advance and then subjected to a surface roughening treatment by pickling. Moreover, the diameter of the die | dye of a small drawing machine used the diameter of 19 mm, and the plug used the semi float type thing whose outer diameter of a straight part is 16.0 mm. The area reduction after cold drawing by the small drawing machine is 43.9%.

Each of the lubricating film forming compositions for plastic working was applied to the steel pipe so that the average film weight after drying was 20 ± 2 g / m ² . Then, the resin layer was formed in the said steel pipe surface by drying at 80 degreeC for 1 hour, and the steel pipe which has the lubricating film for plastic working of this invention was obtained. Thereafter, cold drawing was performed under the above conditions. The non-water type lubricating oil of Comparative Example 5 was applied to the same steel pipe as that used in Examples 1 to 49 with a brush so that it was uniform with a brush. Cold drawing was performed by supplying water-type lubricant. And the performance evaluation was performed by visually observing the surface of the workpiece (steel pipe) after drawing and examining the presence or absence of seizure. The results are also shown in Tables 3 to 6, respectively. “◎” in each table represents that seizure did not occur, “○” represents that very slight seizure occurred, “Δ” represents that slight seizure occurred, “X” represents that severe seizure occurred.

(2) Spike test As a workpiece, an outer diameter of 25 mm, a height of 30 mm, and a cylindrical billet were used.
Each of the lubricating film forming compositions for plastic working was applied to the steel pipe so that the average film weight after drying was 20 ± 2 g / m ² . Then, the resin layer was formed in the said billet surface by drying at 80 degreeC for 1 hour, and the billet which has the lubricating film for plastic working of this invention was obtained. Thereafter, performance was evaluated by a spike test according to the invention of Japanese Patent No. 3227721. The results are also shown in Tables 3 to 6, respectively. “◎” in each table represents that seizure did not occur, “○” represents that slight seizure occurred, “△” represents that half surface seizure occurred, “X” indicates that severe seizure occurred.

[3] Effect of Example When the state of the surface of the steel pipe after the cold drawing process was investigated, in Comparative Examples 1 to 5, which is outside the scope of the present invention, as shown in Table 6, a streak-like burnt surface was formed on the pipe inner surface. A sputum occurred. On the other hand, in Examples 1 to 49 within the scope of the present invention, as shown in Tables 3 to 6, it was confirmed that drawing could be performed without generating surface defects such as seizure. Moreover, in Examples 1 to 49, it was also confirmed that the lubricating coating remaining on the surface of the base material was completely removed by alkali cleaning.

  Further, in the spike test, when the state of the spike test piece after processing was investigated, in Comparative Examples 1 to 5 outside the scope of the present invention, seizure flaws occurred at the spike portion as shown in Table 6. On the other hand, in Examples 1 to 49 within the scope of the present invention, as shown in Tables 3 to 6, it was confirmed that surface flaws such as seizure did not occur. Moreover, as in the cold drawing test, in Examples 1 to 49, it was also confirmed that the lubricating coating remaining on the surface of the base material was completely removed by alkali cleaning.

  The present invention is not limited to the specific examples described above, and can be variously modified examples within the scope of the present invention depending on the purpose and application.

It is explanatory drawing (A) of the process of a plastic working process and the conventional chemical conversion film process, and explanatory drawing (B) of the process of the formation method of the lubricating film for plastic working of this invention.

Claims (21)

A lubricating film for plastic working comprising a resin layer formed on the surface of a base material,
The resin layer contains wax particles, and the resin layer contains 25 to 99 wt% of a resin having a glass transition temperature of 30 ° C. or lower when the resin layer is 100 wt%. Lubricant coating.   2. The lubricating film for plastic working according to claim 1, wherein the resin is at least one of a (meth) acrylic resin, a urethane resin, a polyester resin, a vinyl acetate resin, a polyvinyl alcohol resin, a polyamide resin, and a fluorine resin. .   The wax particles have a solid or viscosity of 10 mPa · s or more at 100 ° C, and the content of the wax particles is 0.5 to 74.5 wt% when the resin layer is 100 wt%. The lubricating film for plastic working according to 1 or 2.   4. The lubricating film for plastic working according to claim 1, wherein the wax particles have an average particle size of 10 μm or less.   The resin layer further contains at least one extreme pressure additive selected from a sulfur-based extreme pressure additive, a phosphorus-based extreme pressure additive, and a chlorine-based extreme pressure additive, and the resin layer is 100 wt%. 5. The lubricating film for plastic working according to claim 1, wherein the content ratio of the extreme pressure additive is 0.5 to 74.5 wt% in terms of solid content.   The lubricating film for plastic working according to any one of claims 1 to 5, wherein the resin layer further contains fine particles having an anti-seizure effect.   When the solvent contains a resin having a glass transition temperature of 30 ° C. or less and wax particles, and the solid content of the composition for forming a lubricating film for plastic working is 100 wt%, the glass transition temperature is A composition for forming a lubricating film for plastic working, wherein the content of a resin at 30 ° C. or lower is 25 to 99 wt%.   The said resin is at least 1 sort (s) among (meth) acrylic-type resin, urethane resin, polyester resin, vinyl acetate resin, polyvinyl alcohol resin, polyamide resin, and fluorine-type resin, Lubricant film formation for plastic working of Claim 7 Composition.   The composition for forming a lubricating film for plastic working according to claim 7, wherein the resin is crosslinked with a compound containing at least one metal element of a typical metal element and a transition metal element and / or ions thereof. .   The composition for forming a lubricating film for plastic working according to claim 7, wherein the resin is a compound containing at least one metal element of a typical metal element and a transition metal element and / or an ionomer crosslinked with ions thereof. .   The plasticity according to claim 9 or 10, wherein the typical metal element is at least one of alkaline earth metal, aluminum, and zinc, and the transition metal element is at least one of iron and copper. A composition for forming a lubricating film for processing.   The wax particles have a solid content or viscosity of 10 mPa · s or more at 100 ° C., and when the solid content of the lubricating film forming composition for plastic working is 100 wt%, the content of the wax particles is 0.00. The composition for forming a lubricating film for plastic working according to any one of claims 7 to 11, which is 5 to 74.5 wt%.   The composition for forming a lubricating film for plastic working according to any one of claims 7 to 12, wherein the wax particles have an average particle size of 10 µm or less.   Solid content of the lubricating film forming composition for plastic working further comprising at least one extreme pressure additive selected from the group consisting of sulfur-based extreme pressure additive, phosphorus-based extreme pressure additive and chlorine-based extreme pressure additive The composition for forming a lubricating film for plastic working according to any one of claims 7 to 13, wherein the content of the extreme pressure additive is 0.5 to 74.5 wt% in terms of solid content when the content is 100 wt%. object.   The composition for forming a lubricating film for plastic working according to any one of claims 7 to 14, further comprising fine particles having an anti-seizure effect.   The composition for forming a lubricating film for plastic working according to claim 15, wherein the fine particles are oxides of at least one metal element of a typical metal element and a transition metal element.   The plastic working according to claim 16, wherein the typical metal element is at least one of alkaline earth metal, aluminum, and zinc, and the transition metal element is at least one of iron and copper. A composition for forming a lubricating film.   The composition for forming a lubricating film for plastic working according to any one of claims 7 to 17, wherein the solvent is water or a solvent containing at least water.   A plastic working material, wherein the plastic working lubricant film according to any one of claims 1 to 6 is formed on a surface of a raw material for producing a plastic working product having an arbitrary shape.   A method for producing a plastically processed product, comprising plastically processing the plastic working material according to claim 19.   A method for producing a metal tube, a metal wire, or a metal rod, wherein the material for plastic working according to claim 19 is drawn.

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