WO2019189136A1 - Composition d'huile de traitement thermique - Google Patents

Composition d'huile de traitement thermique Download PDF

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Publication number
WO2019189136A1
WO2019189136A1 PCT/JP2019/012790 JP2019012790W WO2019189136A1 WO 2019189136 A1 WO2019189136 A1 WO 2019189136A1 JP 2019012790 W JP2019012790 W JP 2019012790W WO 2019189136 A1 WO2019189136 A1 WO 2019189136A1
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Prior art keywords
heat
oil composition
treated oil
seconds
composition according
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PCT/JP2019/012790
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English (en)
Japanese (ja)
Inventor
立樹 本間
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出光興産株式会社
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Application filed by 出光興産株式会社 filed Critical 出光興産株式会社
Priority to JP2020510884A priority Critical patent/JPWO2019189136A1/ja
Priority to CN201980021849.8A priority patent/CN111868269A/zh
Priority to US17/040,790 priority patent/US20210002574A1/en
Publication of WO2019189136A1 publication Critical patent/WO2019189136A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
    • C10M143/16—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing cycloaliphatic monomer
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
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    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/48—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring
    • C10M129/54—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups
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    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/58—Oils
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/003—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions used as base material
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
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    • C10M2205/026—Butene
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/14—Synthetic waxes, e.g. polythene waxes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/26—Overbased carboxylic acid salts
    • C10M2207/262—Overbased carboxylic acid salts derived from hydroxy substituted aromatic acids, e.g. salicylates
    • C—CHEMISTRY; METALLURGY
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    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
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    • C10N2020/011—Cloud point
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    • C10N2020/017—Specific gravity or density
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    • C10N2020/04—Molecular weight; Molecular weight distribution
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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    • C10N2030/04—Detergent property or dispersant property
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/20—Colour, e.g. dyes
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
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    • C10N2040/246—Iron or steel

Definitions

  • the present invention relates to a heat-treated oil composition.
  • quenching is a treatment in which a heated metal material is immersed in a coolant and transformed into a predetermined quenching structure, and the treated product becomes very hard by this quenching.
  • a heated steel material in an austenite state is immersed in a coolant and cooled at an upper critical speed or higher, it can be transformed into a quenched structure such as martensite.
  • an oil-based or water-based heat treatment agent is generally used as the coolant.
  • the quenching of the metal material using the oil-based heat treatment agent (heat treatment oil) will be described.
  • the heated metal material is put into the heat treatment oil as a coolant, it is usually cooled through three stages. Specifically, (1) a first stage (vapor film stage) in which the metal material is covered with a vapor film of heat-treated oil, (2) a second stage (boiling stage) in which the vapor film is broken and boiling occurs, (3) This is a third stage (convection stage) in which the temperature of the metal material is equal to or lower than the boiling point of the heat-treated oil and heat is taken away by convection. In each stage, the cooling rate is different because the atmosphere around the metal material is different, and the cooling rate in the second stage (boiling stage) is the fastest.
  • the cooling rate is rapidly increased when the vaporized film stage is shifted to the boiling stage.
  • the metal material is not a simple planar shape, the vapor film stage and the boiling stage are likely to be mixed on the surface of the metal material.
  • a very large temperature difference is generated on the surface of the metal material due to a difference in cooling rate between the vapor film stage and the boiling stage. And this temperature difference generates thermal stress and transformation stress and causes distortion in the metal material. Therefore, in heat treatment of metal materials, especially quenching, it is important to select heat treatment oils suitable for the heat treatment conditions. If the selection is inappropriate, the metal materials will be distorted and sufficient hardened May not be obtained.
  • the heat-treated oil is classified into 1 to 3 types according to JIS K2242: 2012, and 1 type 1 oil and 2 type oil, 2 types 1 oil and 2 type oil are used for quenching.
  • JISK2242: 2012 the number of cooling seconds from 800 ° C. to 400 ° C. is defined as a measure of cooling performance.
  • Type 1 No. 1 is 5.0 seconds or less
  • Type 1 No. 2 is 4.0 seconds or less
  • Type 2 No. 2 is set to 6.0 seconds or less.
  • the shorter the cooling time the higher the cooling performance and the harder the metal material.
  • the hardness and strain of a metal after quenching are in a trade-off relationship, and the harder the strain, the greater the strain.
  • the number of seconds at 300 ° C. is also used as an index indicating the cooling property of the oil.
  • the number of seconds at 300 ° C. is a cooling time from 800 ° C. to 300 ° C. of the cooling curve obtained in accordance with the cooling performance test method of JIS K2242: 2012.
  • the number of seconds (characteristic seconds; vapor film length) until reaching the temperature (characteristic temperature) from the start to the end of the vapor film stage is also used as an index indicating the cooling property of the oil agent.
  • the characteristic temperature is also defined, Type 1 No. 1 is 480 ° C or higher, Type 1 No. 2 is 580 ° C or higher, Type 2 No. 1 is 500 ° C or higher, and Type 2 No. 2 is 600 ° C or higher. It has been established.
  • These 1 type 1 and 2 oils correspond to cold oils used at low oil temperatures, and 2 types 1 oils correspond to semi-hot oils that can be used at higher oil temperatures. Oil corresponds to hot oil that can be used at high oil temperatures.
  • the user selects the quenching oil based on the above indicators in order to obtain the desired hardness and distortion.
  • the above-mentioned Type 2 No. 1 oil is widely used for quenching of gear parts for automobiles in which distortion is a problem. This is because the above-mentioned type 1 oil increases the strain and, depending on the part, the hardness is too high. In addition, although the type 2 No. 2 oil has less strain, the hardness is insufficient.
  • variation in the cooling performance at the time of group quenching having cooling performance comparable as the said 2 type 1 oil.
  • a heat-treated oil composition comprising a mixed base oil comprising more than 95%.
  • kinematic viscosity of 5 mm 2 / s to 60 mm 2 / s is 50% by mass to 95% by mass based on the total amount of the composition, and a 40 ° C. kinematic viscosity is 300 mm 2 / s or more.
  • a heat-treated oil composition is proposed that can reduce variation in cooling performance during group quenching by blending 5% by mass to 50% by mass of the base oil, based on the total amount of the composition, and an ⁇ -olefin copolymer. ing.
  • Patent Document 3 includes a petroleum resin as a vapor film breaker as a heat-treating oil composition that reduces the variation in cooling performance during group quenching while having the same cooling performance as Type 2 No. 1 oil.
  • a heat-treated oil composition has been proposed in which the number is 1.00 seconds or less and the 300 ° C. seconds are 6.00 seconds or more and 14.50 seconds or less.
  • Patent Document 4 an alkenyl or alkyl succinimide is blended with a base oil having a kinematic viscosity at 40 ° C. of 4 mm 2 / s or more and 20 mm 2 / s or less as a heat-treated oil composition that can exhibit high cooling performance.
  • Heat treated oil compositions have been proposed.
  • the present invention is as follows. [1] comprising (A) a base oil and (B) a vapor film breaker; The cooling time obtained from 800 ° C. to 300 ° C. of the cooling curve obtained in accordance with the cooling performance test method of JIS K2242: 2012 is 6.5 seconds or more and less than 10 seconds,
  • the component (B) is a heat-treated oil composition containing a petroleum resin.
  • the petroleum resin is at least one unsaturated compound selected from aliphatic olefins having 4 to 10 carbon atoms, aliphatic diolefins, and aromatic compounds having 8 or more carbon atoms having an olefinically unsaturated bond.
  • the heat-treated oil composition according to any one of [1] to [7], wherein the compound is a polymerized or copolymerized resin.
  • the petroleum resin includes an aliphatic petroleum resin, an aromatic petroleum resin, an aliphatic-aromatic copolymer petroleum resin, a dicyclopentadiene petroleum resin, and a dicyclopentadiene-aromatic copolymer petroleum resin.
  • the component (A), a high viscosity base oil is a low viscosity base oil and 40 ° C. kinematic viscosity 40 ° C. kinematic viscosity of less than 1 mm 2 / s or more 85 mm 2 / s is 85 ⁇ 550mm 2 / s
  • a heat treated oil composition having a good balance of cooling performance, quenching hardness, and quenching strain.
  • the present invention relates to a heat-treated oil composition
  • a heat-treated oil composition comprising (A) a base oil and (B) a vapor film breaker.
  • the heat-treated oil composition of the present invention has a cooling time of 300 ° C., which is a cooling time from 800 ° C. to 300 ° C. of the cooling curve obtained according to the cooling performance test method of JIS K2242: 2012, which is 6.5 seconds.
  • the component (B) contains a petroleum resin.
  • the heat-treated oil composition of the present invention is excellent in the balance of cooling performance, quenching hardness, and quenching strain.
  • the heat-treated oil compositions described in Patent Documents 1 to 3 have a long cooling time and a reduced quenching strain.
  • the quenching hardness may be insufficient for application to transportation parts such as automobile parts (for example, gears and bearings), and a further increase in hardness is required.
  • the heat-treated oil composition described in Patent Document 4 Japanese Patent Application Laid-Open No. 2010-229479
  • the heat-treated oil composition of a preferred embodiment can achieve improved quenching hardness while suppressing quenching strain and variation in strain.
  • the heat-treated oil composition of the embodiment can be suitably used in group quenching of parts because quenching strain and variation in strain are suppressed.
  • the heat-treated oil composition of this embodiment can be suitably used for transportation parts such as automobile parts (for example, gears and bearings), particularly small parts.
  • transportation parts such as automobile parts (for example, gears and bearings), particularly small parts.
  • each component will be described in detail.
  • the upper limit value and the lower limit value of the numerical ranges described in this specification can be arbitrarily combined. For example, when “A to B” and “C to D” are described, the ranges of “A to D” and “C to B” are also included in the scope of the present invention. Further, the numerical range “lower limit value to upper limit value” described in the present specification means that the value is not less than the lower limit value and not more than the upper limit value.
  • Base oil There is no restriction
  • Mineral oil includes wax (gas) produced by paraffin-based mineral oil, intermediate-based mineral oil, naphthenic-based mineral oil, etc. obtained by ordinary refining methods such as solvent refining and hydrogenation refining, or Fischer-Tropsch process. (Turi Liquid Wax) and mineral oil-based waxes. These mineral oils may be used alone or in combination of two or more. Mineral oil is classified into group 1, 2, or 3 in the API (American Petroleum Institute) base oil category. The mineral oil is preferably a mineral oil classified into Group 2 and Group 3 of the base oil category, and more preferably a mineral oil classified into Group 3.
  • Examples of synthetic oils include hydrocarbon synthetic oils and ether synthetic oils.
  • Examples of the hydrocarbon-based synthetic oil include alkylbenzene and alkylnaphthalene.
  • Examples of ether synthetic oils include polyoxyalkylene glycol and polyphenyl ether. These synthetic oils may be used alone or in combination of two or more. Further, as the base oil, one or more mineral oils and one or more synthetic oils may be used in combination.
  • the viscosity of the base oil is preferably 40 to 500 mm 2 / s, more preferably 50 to 350 mm 2 / s, still more preferably 60 to 200 mm 2 / s, and more preferably 80 to It is especially preferable that it is 120 mm ⁇ 2 > / s.
  • the base oil of a component (A) is a base oil with which 2 or more types of base oils were mixed, it is preferable that dynamic viscosity of mixed base oil satisfy
  • the kinematic viscosity at a predetermined temperature means a value measured according to JIS K2283: 2000.
  • the content of the base oil is preferably 10 to 99.9% by mass, more preferably 50 to 99% by mass, still more preferably 70 to 97% by mass, based on the total amount of the composition. It is particularly preferably 85 to 95% by mass.
  • the base oil has a kinematic viscosity at 40 ° C. of 1 mm 2 / s or more and less than 85 mm 2 / s (more preferably 20 to 82 mm 2 / s, more preferably 40 to 80 mm 2 / s).
  • the blending of the low-viscosity base oil and the high-viscosity base oil in the mixed base oil is performed by adding the low-viscosity base oil in the heat-treated oil composition in an amount of 0% by mass or more and less than 50% by mass (more preferably 3-30). It is preferable to contain 50% to 99.9% by mass (more preferably 65 to 95% by mass, still more preferably 80 to 90% by mass) of the high-viscosity base oil.
  • the base oil has a low viscosity having a kinematic viscosity at 40 ° C. of 1 to 90 mm 2 / s (more preferably 20 to 82 mm 2 / s, more preferably 40 to 80 mm 2 / s). And a base oil and a high-viscosity base oil having a kinematic viscosity at 40 ° C. of 90 to 500 mm 2 / s (more preferably 88 to 520 mm 2 / s, still more preferably 90 to 490 mm 2 / s).
  • the blending of the low-viscosity base oil and the high-viscosity base oil in the mixed base oil is performed by adding the low-viscosity base oil in the heat-treated oil composition in an amount of 0% by mass or more and less than 50% by mass (more preferably 3-30). It is preferable to contain 50% to 99.9% by mass (more preferably 65 to 95% by mass, still more preferably 80 to 90% by mass) of the high-viscosity base oil.
  • the heat-treated oil composition contains a petroleum resin as a vapor film breaker.
  • a petroleum resin as a vapor film breaker.
  • the vapor film stage can be shortened, and it is difficult to mix the vapor film stage and the boiling stage on the surface of the metal material.
  • variations in cooling performance (hardness and distortion variations) for each component can be made difficult to occur during quenching.
  • even in the case of a component having a complicated shape it is difficult to cause variation in cooling performance for each location of the component, so that distortion of each component can be suppressed.
  • the characteristic seconds in the initial stage of the heat treatment can be shortened, whereby excellent cooling performance can be imparted from the initial stage of the heat treatment.
  • the life of the heat-treated oil composition can be extended by using a petroleum resin.
  • the reason why the petroleum resin can exert these effects is considered to be the thermoplasticity of the petroleum resin and the excellent solubility in the base oil.
  • Petroleum resin is an aliphatic olefin or aliphatic diolefin having 4 to 10 carbon atoms or carbon number having an olefinic unsaturated bond obtained as a by-product during the production of olefins such as ethylene by thermal decomposition of petroleum such as naphtha. It is a resin obtained by polymerizing or copolymerizing one or two or more unsaturated compounds selected from eight or more aromatic compounds.
  • a petroleum resin is a resin (dicyclopentadiene-aromatic copolymer petroleum resin) obtained by copolymerizing an unsaturated compound containing dicyclopentadiene and an aromatic compound, the main raw material of which is a C5 fraction.
  • These petroleum resins include, for example, “aliphatic petroleum resins” obtained by polymerizing aliphatic olefins and / or aliphatic diolefins, and “aromatic petroleum resins obtained by polymerizing aromatic compounds having olefinic unsaturated bonds. And “aliphatic-aromatic copolymer petroleum resin” obtained by copolymerizing aliphatic olefins and / or aliphatic diolefins with an aromatic compound having an olefinically unsaturated bond. Examples of the aliphatic olefins having 4 to 10 carbon atoms include butene, pentene, hexene, heptene and the like.
  • Examples of the aliphatic diolefin having 4 to 10 carbon atoms include butadiene, pentadiene, isoprene, cyclopentadiene, dicyclopentadiene, and methylpentadiene.
  • Examples of the aromatic compound having 8 or more carbon atoms having an olefinically unsaturated bond include styrene, ⁇ -methylstyrene, ⁇ -methylstyrene, vinyltoluene, vinylxylene, indene, methylindene, and ethylindene.
  • dicyclopentadiene-based petroleum resin obtained by polymerization of cyclopentadiene or dicyclopentadiene (DCPD), or by copolymerizing these cyclopentadiene or dicyclopentadiene with an aromatic compound having an olefinically unsaturated bond.
  • DCPD dicyclopentadiene
  • dicyclopentadiene-aromatic copolymer petroleum resin for example, dicyclopentadiene-styrene petroleum resin
  • petroleum resin includes derivatives of petroleum resin such as hydrogenated petroleum resin and modified petroleum resin.
  • the hydrogenated petroleum resin is a hydrogenated petroleum resin obtained by adding hydrogen atoms to the above petroleum resin. By hydrogenation, all or some of the double bonds in the molecule are hydrogenated. Accordingly, the hydrogenated petroleum resin may be a fully hydrogenated petroleum resin or a partially hydrogenated petroleum resin. When a partially hydrogenated product is used, it is easy to manufacture because of excellent cooling properties and a low softening point.
  • the modified petroleum resin include an acid-modified petroleum resin obtained by modifying the petroleum resin with an acidic functional group typified by carboxylic acid, and the acid-modified petroleum resin using a compound such as alcohol, amine, alkali metal, or alkaline earth metal.
  • Reaction-modified resins are exemplified.
  • the acid-modified petroleum resin include a carboxylic acid-modified petroleum resin obtained by modifying a petroleum resin with an unsaturated carboxylic acid or an unsaturated carboxylic acid anhydride, and an acid anhydride-modified petroleum resin.
  • unsaturated carboxylic acids include unsaturated monocarboxylic acids such as acrylic acid and methacrylic acid; unsaturated polycarboxylic acids such as maleic acid, fumaric acid, itaconic acid, and citraconic acid; monomethyl maleate, monoethyl fumarate, etc.
  • unsaturated carboxylic acid anhydrides include unsaturated polyvalent carboxylic acid anhydrides such as maleic anhydride and itaconic anhydride.
  • a petroleum resin a synthesized resin or a commercially available product may be used.
  • a petroleum resin may be used independently and may be used in combination of 2 or more type.
  • the petroleum resin is an aliphatic petroleum resin, an aromatic petroleum resin, an aliphatic-aromatic copolymer petroleum resin, a dicyclopentadiene petroleum resin, and a dicyclopentadiene-aromatic copolymer petroleum.
  • Resin and at least one selected from hydrogenated petroleum resins and modified petroleum resins.
  • the petroleum resin is preferably an aliphatic-aromatic copolymer petroleum resin or a hydrogenated aliphatic-aromatic copolymer petroleum resin from the viewpoint that the characteristic seconds can be shortened.
  • An added aliphatic-aromatic copolymer petroleum resin is preferred.
  • the petroleum resin is a dicyclopentadiene-aromatic copolymer hydrogenated petroleum resin.
  • the number average molecular weight (Mn) of the petroleum resin is preferably 200 to 5000, more preferably 250 to 2500, and further preferably 300 to 1500 in terms of characteristic seconds.
  • the number average molecular weight (Mn) can be measured by the VPO method.
  • the petroleum resin preferably has a softening point of 40 ° C or higher, more preferably 40 ° C or higher and 150 ° C or lower, still more preferably 60 ° C or higher and 150 ° C or lower, and 80 ° C or higher and 140 ° C or lower. More preferably, it is more preferably 100 ° C. or higher and 135 ° C. or lower, and particularly preferably 120 ° C. or higher and 130 ° C. or lower.
  • the “softening point” can be measured by the ring and ball method of JIS K2207: 2006. By setting the softening point to 40 ° C.
  • the softening point of the petroleum resin can be adjusted by the degree of polymerization of the petroleum resin, the modifying component, and the degree of modification. In addition, when using 2 or more types of materials as petroleum resin, it is preferable that all the materials are the range of the said softening point.
  • the petroleum resin preferably has a density at 20 ° C. of 0.5 to 1.5 g / cm 3 measured in accordance with JIS K 0061: 2001 from the viewpoint of cooling performance, and preferably 0.7 to 1. More preferably, it is 3 g / cm 3 , and even more preferably 0.8 to 1.1 g / cm 3 .
  • the bromine number of the petroleum resin is preferably 30 g / 100 g or less, more preferably 20 g / 100 g or less, and even more preferably 10 g / 100 g or less from the viewpoint of cooling performance.
  • the lower the bromine value the better.
  • the lower limit is not particularly limited, but is usually 1.0 g / 100 g or more, 1.5 g / 100 g or more, or 1.9 g / 100 g or more.
  • the bromine number is measured in accordance with JIS K 2605: 1996.
  • the Hazen color number measured in accordance with JIS K 6901: 2008 is preferably 50 or less, more preferably 40 or less, and even more preferably 30 or less.
  • the lower limit is not particularly limited, but is usually 3 or more, 5 or more, or 7 or more.
  • the content of petroleum resin is preferably 0.1 to 90% by mass based on the total amount of the composition. If it is 0.1 mass% or more, the cooling performance can be improved. Petroleum resins generally have a high viscosity, and the viscosity of the composition tends to increase as the blending amount increases. If it is 90 mass% or less, it is preferable from the point of appropriate viscosity.
  • the content of the petroleum resin is more preferably 1 to 60% by mass, and still more preferably 5 to 10% by mass from the viewpoint of appropriate viscosity and cooling performance.
  • the heat-treated oil composition may contain a vapor film breaker other than petroleum resin.
  • Other vapor film breakers include terpene resins, terpene resin derivatives, rosin, rosin derivatives, and the like.
  • the content of the other vapor film breaking agent is preferably 30% by mass or less, more preferably 20% by mass or less, and still more preferably 10% by mass or less, based on the total amount of the composition.
  • the heat-treated oil composition does not contain a vapor film breaker other than petroleum resin.
  • the heat-treated oil composition of one embodiment does not contain an ⁇ -olefin copolymer as a vapor film breaker.
  • the heat-treated oil composition of one embodiment does not contain asphalt as a vapor film breaker.
  • the heat-treated oil composition may contain a metal-based cleaning dispersant. Cooling performance can be improved by including a metallic detergent-dispersant. By including (D) a metal-based detergent / dispersant together with (B) a petroleum resin used as a vapor film breaker, excellent cooling performance can be exhibited, and a further improvement effect of hardness during quenching can be obtained.
  • Examples of the (C) metallic detergent-dispersant include organometallic compounds containing a metal atom (preferably an alkaline earth metal atom) selected from alkali metal atoms and alkaline earth metal atoms. Include metal salicylates, metal phenates, metal sulfonates, and the like. As a metal atom, a sodium atom, a calcium atom, a magnesium atom, or a barium atom is preferable, a calcium atom or a magnesium atom is more preferable, and a calcium atom is more preferable. That is, in one embodiment, (C) the metal-based detergent dispersant includes at least one of calcium salicylate, calcium phenate, and calcium sulfonate. A metal type detergent dispersing agent may be used independently and may be used in combination of 2 or more type.
  • the content of the metal-based detergent dispersant is preferably 0 to 10% by mass, more preferably 0.1 to 7.5% by mass, and further preferably 0.5 to 5% by mass based on the total amount of the composition. .
  • the above range is preferable from the viewpoint of dispersibility in base oil and excellent cooling performance.
  • the heat-treated oil composition may further contain other additives such as an antioxidant and a glitter improvement agent.
  • the content of other additives is preferably 10% by mass or less, more preferably 0.01 to 5% by mass, based on the composition.
  • antioxidant As an antioxidant, arbitrary things can be suitably selected and used from well-known antioxidant used as an antioxidant of the heat processing oil composition conventionally. For example, an amine antioxidant, a phenolic antioxidant, etc. are mentioned.
  • amine antioxidants include diphenylamine and diphenylamine antioxidants such as alkylated diphenylamine having an alkyl group having 3 to 20 carbon atoms; ⁇ -naphthylamine, alkyl substituted phenyl- ⁇ -naphthylamine having 3 to 20 carbon atoms, and the like. Naphthylamine antioxidants, and the like.
  • phenolic antioxidant examples include 2,6-di-tert-butyl-4-methylphenol, 2,6-di-tert-butyl-4-ethylphenol, and octadecyl-3- (3,5-diphenol).
  • Monophenol antioxidants such as -tert-butyl-4-hydroxyphenyl) propionate; 4,4'-methylenebis (2,6-di-tert-butylphenol), 2,2'-methylenebis (4-ethyl-6) -Tert-butylphenol) and the like; hindered phenol antioxidants; and the like.
  • antioxidants may be used alone or in combination of two or more.
  • the content of the antioxidant is preferably 0.01 to 10% by mass, more preferably 0.03 to 5% by mass, and still more preferably 0.05 to 3% by mass, based on the total amount of the composition.
  • the glitter improvement agent can improve the appearance of the object to be processed.
  • the glitter improving agent include fats and oils, fatty oils and fatty acids, alkenyl succinimides, substituted hydroxyaromatic carboxylic acid ester derivatives, and the like. These glitter improvement agents may be used alone or in combination of two or more.
  • the content of the glitter improving agent is preferably 0.01 to 5% by mass, more preferably 0.02 to 3% by mass, based on the total amount of the composition.
  • the total content of (A) the base oil and (B) the vapor film breaker in the heat-treated oil composition is 80 to 100% by mass based on the total amount of the composition (100% by mass). It is preferably 90 to 99.5% by mass, more preferably 97 to 99% by mass. In one embodiment of the present invention, the total content of (A) base oil, (B) vapor film breaker, and (C) glitter improvement agent in the heat-treated oil composition is the total amount of the composition (100% by mass).
  • the reference is preferably 90 to 100% by mass, more preferably 95 to 100% by mass, and particularly preferably 97.5 to 100% by mass.
  • the heat-treated oil composition of the present embodiment has a “300 ° C. second” that is a cooling time from 800 ° C. to 300 ° C. of the cooling curve obtained in accordance with the cooling performance test method of JIS K2242: 2012. It must be 5 seconds or more and less than 10 seconds.
  • the number of seconds at 300 ° C. is more preferably 6.6 seconds or more and 9.5 seconds or less, and further preferably 6.8 seconds or more and 9.2 seconds or less, from the viewpoint of achieving both quenching hardness, strain, and variations thereof. In order to set the 300 ° C.
  • the heat-treated oil composition having 300 ° C. seconds in the above range can be used as a heat-treated oil (semi-hot oil) having a cooling performance comparable to that of Type 2 No. 1 oil in JIS K2242: 2012.
  • the heat-treated oil composition of the embodiment can realize quenching distortion variation and high quenching hardness as compared with conventional semi-hot oil.
  • the heat-treated oil composition of one embodiment is a cooling time from 800 ° C. to 400 ° C. of the cooling curve obtained according to the cooling performance test method of JIS K2242: 2012 from the viewpoint of cooling performance “400
  • the “° C. seconds” is preferably 2.0 to 4.5 seconds, more preferably 2.25 to 4.0 seconds, and even more preferably 2.3 to 3.5 seconds.
  • the heat-treated oil composition of the present embodiment has a characteristic number of seconds (vapor film length) obtained from a cooling curve obtained in accordance with a cooling performance test method of JIS K2242: 2012 from the viewpoint of reducing strain and variation. Is preferably 1 second or longer, more preferably 1.2 seconds or longer, and particularly preferably 1.3 seconds or longer. Further, from the viewpoint of reducing variation in cooling performance for each part during quenching, it is preferably 10 seconds or less, more preferably 5 seconds or less, and even more preferably 2.5 seconds or less.
  • the characteristic seconds (vapor film length) obtained from the cooling curve is 1 second to 10 seconds, 1 second to 5 seconds, 1 second to 2.5 seconds, 1.2 seconds to 10 seconds, 1.2 seconds to 5 seconds, 1.2 seconds to 2.5 seconds, 1.3 seconds to 10 seconds, 1.3 seconds to 5 seconds, or 1.3 seconds to 2.5 seconds is there.
  • (B) vapor film breaker (particularly petroleum resin) content, softening point and number average It is preferable that the molecular weight, the content and structure of the (C) metal-based detergent / dispersant are within the range of the above-described embodiment.
  • the characteristic number of seconds can be calculated by the following (1) and (2).
  • (1) In accordance with the cooling performance test method of JIS K2242: 2012, a silver sample heated to 810 ° C. is charged into the heat-treated oil composition, and cooling is performed with time as the x axis and the temperature of the silver sample surface as the y axis. Find a curve.
  • the measurement time interval is preferably 1/100 second.
  • the kinematic viscosity at 40 ° C. heat treatment oil composition from the viewpoint of 300 ° C. seconds, preferably 10 ⁇ 280mm 2 / s, more preferably 10 ⁇ 200mm 2 / s, or, 65 ⁇ 230mm 2 / s Gayori 115 to 180 mm 2 / s is more preferable.
  • the kinematic viscosity at 100 ° C. heat treatment oil composition from the viewpoint of 300 ° C. seconds, preferably 1 ⁇ 40mm 2 / s, more preferably 5 ⁇ 30mm 2 / s, more preferably 10 ⁇ 20mm 2 / s.
  • the manufacturing method of the heat-treated oil composition of the embodiment is not particularly limited.
  • the production method of the embodiment includes mixing (A) a base oil and (B) a vapor film breaker, and (C) a metal-based detergent dispersant and (D) other components as necessary.
  • the components (A) to (D) may be blended by any method, and the blending order and method are not limited.
  • the heat-treated oil composition of the embodiment can exhibit excellent cooling performance in heat treatment of metal materials, and therefore, for example, various alloy steels such as carbon steel, nickel-manganese steel, chromium-molybdenum steel, and manganese steel are quenched. It can be suitably used as the heat treatment oil at the time.
  • the heat-treated oil composition of the embodiment can achieve improved quenching hardness while suppressing quenching distortion, for example, gears such as gears for automobiles, quenching oil used for group quenching of metal materials, etc. Can be suitably used.
  • the temperature range of the heat-treated oil composition when quenching a metal material using the heat-treated oil composition of the embodiment may be set to a range of 60 to 150 ° C., which is a normal quenching temperature.
  • the temperature may be set at a high temperature of 170 to 250 ° C.
  • One embodiment of the present invention provides a method for heat treating a metal material. Specifically, the heat treatment method includes heat-treating a metal material using the heat-treated oil composition of the above embodiment.
  • One embodiment of the present invention provides a method for quenching a metal material. Specifically, the metal material is treated using the heat-treated oil composition of the above embodiment.
  • the method for quenching a metal material is characterized in that the metal material is treated using the heat-treated oil composition of the above embodiment in the group quenching of the metal material.
  • One embodiment of the present invention provides a method for group quenching of a metal material, comprising treating the metal material with the heat-treated oil composition of the above-described embodiment.
  • the method for quenching a metal material includes treating the metal material under an oil temperature of 60-200 ° C.
  • Examples 1 and 2 Comparative Examples 1 to 7
  • Table 1 each component shown in Table 1 below was blended with the base oil to prepare base oil and heat-treated oil compositions of Examples and Comparative Examples containing these components, and the heat treatment prepared
  • the oil composition was evaluated for the following hardness and strain.
  • the properties and evaluation results of the heat-treated oil compositions of Examples and Comparative Examples are shown in Table 1 below.
  • Base oil component (A)
  • Base oil 1 paraffinic mineral oil (kinematic viscosity at 40 ° C. 480 mm 2 / s) (high viscosity base oil)
  • Base oil 2 paraffinic mineral oil (40 ° C. kinematic viscosity 75 mm 2 / s) (low viscosity base oil)
  • Base oil 3 paraffinic mineral oil (40 ° C. kinematic viscosity 97 mm 2 / s) (high viscosity base oil)
  • Base oil 4 paraffinic mineral oil (40 ° C.
  • Base oil 5 paraffinic mineral oil (40 ° C. kinematic viscosity 395 mm 2 / s) (high viscosity base oil)
  • Base oil 6 Paraffinic mineral oil (40 ° C. kinematic viscosity 31 mm 2 / s) (low viscosity base oil)
  • Base oil 7 paraffinic mineral oil (40 ° C. kinematic viscosity 14 mm 2 / s) (low viscosity base oil)
  • Base oil 8 paraffinic mineral oil (40 ° C.
  • Base oil 9 paraffinic mineral oil (40 ° C. kinematic viscosity 120 mm 2 / s) (high viscosity base oil)
  • Base oil 10 Paraffinic mineral oil (40 ° C. kinematic viscosity 60 mm 2 / s) (low viscosity base oil)
  • Base oil 11 Paraffinic mineral oil (40 ° C. kinematic viscosity 200 mm 2 / s) (high viscosity base oil) 2.
  • Petroleum resin 1 Fully hydrogenated aliphatic-aromatic copolymer petroleum resin (dicyclopentadiene-aromatic copolymer hydrogenated petroleum resin mainly containing C5 fraction; softening point: 125 ° C, number average Molecular weight: 820, density at 20 ° C .: 1.03 g / cm 3 , hue (Hazen color number): 20, bromine number: 2.5 g / 100 g)
  • Petroleum resin 2 Partially hydrogenated aliphatic-aromatic copolymer petroleum resin (dicyclopentadiene-aromatic copolymer hydrogenated petroleum resin with C5 fraction as main raw material; softening point: 110 ° C., number average Molecular weight: 760, density at 20 ° C .: 1.05 g / cm 3 , hue (Hazen color number): 25, bromine number: 6 g / 100 g) ⁇ -olefin copolymer: ⁇ -
  • the heat-treated oil composition of the example containing a petroleum resin as a vapor film breaker and having a 300 ° C. seconds of 6.5 seconds or more and less than 10 seconds has an average of 400 Hv or more. It was confirmed that it had an internal hardness and an average effective hardening depth of 1.0 mm or more, and that the average ellipticity (less than 0.21) and its variation (ellipticity 3 ⁇ less than 0.18) were small. . On the other hand, when the number of seconds at 300 ° C.
  • Comparative Example 5 to 7 where the number of seconds at 300 ° C. exceeds 10 seconds, the average internal hardness is less than 350 Hv.
  • Comparative Example 4 in which the number of seconds at 300 ° C. is less than 6.5 seconds and no petroleum resin is included, and in Comparative Examples 1 and 2 that do not include a petroleum resin, quenching strain (particularly, variation in quenching strain (ellipticity 3 ⁇ )) is observed. It was big.
  • the heat-treated oil composition of the present invention can be suitably used for heat treatment such as quenching of a metal material.

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Abstract

L'invention concerne une composition d'huile de traitement thermique qui permet de supprimer la distorsion de refroidissement et la variation de distorsion, et d'obtenir une dureté de refroidissement améliorée. L'invention concerne une composition d'huile de traitement thermique qui comprend une huile de base (A) et un agent de rupture de film de vapeur (B). La composition d'huile de traitement thermique fait en sorte que, sur une courbe de refroidissement obtenue conformément au procédé de test de performance de refroidissement dans JIS K2242:2012, le temps en secondes pour atteindre 300 °C, par exemple, le temps de refroidissement de 800 °C à 300 °C, est d'au moins 6,5 secondes mais inférieur à 10 secondes. Le composant (B) comprend une résine de pétrole.
PCT/JP2019/012790 2018-03-28 2019-03-26 Composition d'huile de traitement thermique WO2019189136A1 (fr)

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WO2007000976A1 (fr) * 2005-06-28 2007-01-04 Idemitsu Kosan Co., Ltd. Composition d'huile pour traitement thermique
WO2016133093A1 (fr) * 2015-02-18 2016-08-25 出光興産株式会社 Composition d'huile de traitement thermique
WO2016132860A1 (fr) * 2015-02-18 2016-08-25 出光興産株式会社 Composition d'huile de traitement thermique

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AU2002357258A1 (en) * 2001-12-18 2003-06-30 The Lubrizol Corporation Quenching oil compositions
JP5253772B2 (ja) * 2007-07-27 2013-07-31 出光興産株式会社 熱処理油組成物
US11035015B2 (en) * 2015-01-21 2021-06-15 Idemitsu Kosan Co., Ltd. Vapor film-rupturing agent, and thermal treatment oil composition
CN107151728B (zh) * 2017-05-08 2018-11-02 三河市炬峰生物能源有限公司 一种转基因大豆油型金属热处理淬火油及其制备方法

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WO2007000976A1 (fr) * 2005-06-28 2007-01-04 Idemitsu Kosan Co., Ltd. Composition d'huile pour traitement thermique
WO2016133093A1 (fr) * 2015-02-18 2016-08-25 出光興産株式会社 Composition d'huile de traitement thermique
WO2016132860A1 (fr) * 2015-02-18 2016-08-25 出光興産株式会社 Composition d'huile de traitement thermique

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