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EP3677661A1 - Schmierfettzusammensetzung - Google Patents

Schmierfettzusammensetzung Download PDF

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Publication number
EP3677661A1
EP3677661A1 EP18850947.5A EP18850947A EP3677661A1 EP 3677661 A1 EP3677661 A1 EP 3677661A1 EP 18850947 A EP18850947 A EP 18850947A EP 3677661 A1 EP3677661 A1 EP 3677661A1
Authority
EP
European Patent Office
Prior art keywords
grease composition
grease
concave
urea
group
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP18850947.5A
Other languages
English (en)
French (fr)
Other versions
EP3677661A4 (de
Inventor
Go Watanabe
Akihiro Shishikura
Asami KOGA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Idemitsu Kosan Co Ltd
Original Assignee
Idemitsu Kosan Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Idemitsu Kosan Co Ltd filed Critical Idemitsu Kosan Co Ltd
Publication of EP3677661A1 publication Critical patent/EP3677661A1/de
Publication of EP3677661A4 publication Critical patent/EP3677661A4/de
Withdrawn legal-status Critical Current

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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
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • 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
    • 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
    • C10M169/06—Mixtures of thickeners and additives
    • 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
    • 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
    • C10M129/68—Esters
    • C10M129/76—Esters containing free hydroxy or carboxyl 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
    • 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
    • C10M171/06—Particles of special shape or size
    • 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
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • 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
    • 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
    • C10M2207/28—Esters
    • C10M2207/287—Partial esters
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/287—Partial esters
    • C10M2207/289—Partial esters containing free 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/02—Viscosity; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/046—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for traction drives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • urea-based grease using a urea-based thickener has a long lubricating life at a high temperature and is excellent in oxidation stability, heat resistance, and water resistance.
  • the present inventors focused on the particle size distribution of particles containing urea-based thickener in a grease composition containing a base oil, a urea-based thickener, an antioxidant, and a rust inhibitor.
  • aggregates which are composed only of additives such as the antioxidant (C) and the rust inhibitor (D) and which do not contain the urea-based thickener (B) are excluded from the above-mentioned "particles containing the urea-based thickener (B)".
  • excludeded means that aggregates composed only of additives such as the antioxidant (C) and the rust inhibitor (D) are very small in comparison with the "particles containing the urea-based thickener (B)", so that they are hardly detected in the measurement of particle size with light scattering, and are negligible even if they are detected.
  • the particle size indicating the maximum frequency of the peak is 1.0 ⁇ m or less.
  • the particle size is an index indicating the degree of aggregation of the urea-based thickener (B).
  • Examples of the mineral oil include a distillate oil obtained by atmospheric distillation or vacuum distillation of paraffin crude oil, intermediate base crude oil, or naphthenic crude oil, and a refined oil obtained by refining these distillate oils according to a conventional method.
  • refining process examples include solvent dewaxing treatment, hydroisomerization treatment, hydrofinishing treatment, and clay treatment.
  • Examples of the synthetic oil include a hydrocarbon oil, an aromatic oil, an ester oil, an ether oil, a synthetic oil obtained by isomerizing a wax (GTL wax) produced by Fischer-Tropsch process, or the like.
  • ether oil examples include polyglycols such as polyethylene glycol, polypropylene glycol, polyethylene glycol monoether, and polypropylene glycol monoether; phenyl ether oils such as monoalkyl triphenyl ether, alkyl diphenyl ether, dialkyl diphenyl ether, pentaphenyl ether, tetraphenyl ether, monoalkyl tetraphenyl ether, and dialkyl tetraphenyl ether.
  • polyglycols such as polyethylene glycol, polypropylene glycol, polyethylene glycol monoether, and polypropylene glycol monoether
  • phenyl ether oils such as monoalkyl triphenyl ether, alkyl diphenyl ether, dialkyl diphenyl ether, pentaphenyl ether, tetraphenyl ether, monoalkyl tetraphenyl ether, and dialkyl tetraphenyl ether.
  • the kinematic viscosity at 40°C of the base oil (A) used in one embodiment of the present invention is preferably 10 to 130 mm 2 /s, more preferably 15 to 110 mm 2 /s, and still more preferably 20 to 100 mm 2 /s.
  • the viscosity index of the base oil (A) used in one embodiment of the present invention is preferably 60 or more, more preferably 70 or more, and still more preferably 80 or more.
  • kinematic viscosity and the viscosity index mean values measured in accordance with JIS K2283:2003.
  • the urea-based thickener (B) contained in the grease composition of the present invention may be a compound having a urea bond, but is preferably a diurea having two urea bonds, and more preferably a compound represented by the following general formula (b1).
  • the urea-based thickener (B) used in one embodiment of the present invention may be composed of one type or a mixture of two or more types.
  • Examples of the monovalent hydrocarbon groups that can be selected as R 1 and R 2 include saturated or unsaturated monovalent chain hydrocarbon groups, saturated or unsaturated monovalent alicyclic hydrocarbon groups, and monovalent aromatic hydrocarbon groups, and preferably saturated or unsaturated monovalent chain hydrocarbon groups.
  • Examples of monovalent saturated chain hydrocarbon groups include straight-chain or branched-chain alkyl groups having 6 to 24 carbon atoms, and specific examples include a hexyl group, a heptyl group, an octyl group, a nonyl group, a decyl group, an undecyl group, a dodecyl group, a tridecyl group, a tetradecyl group, a pentadecyl group, a hexadecyl group, a heptadecyl group, an octadecyl group, an octadecenyl group, a nonadecyl group, and an icosyl group.
  • the monovalent saturated chain hydrocarbon group and monovalent unsaturated chain hydrocarbon group may be a straight chain group or a branched chain group.
  • Examples of monovalent saturated alicyclic hydrocarbon groups include cycloalkyl groups, such as a cyclohexyl group, a cycloheptyl group, a cyclooctyl group, and a cyclononyl group; and cycloalkyl groups substituted with an alkyl group having 1 to 6 carbon atoms (preferably cyclohexyl groups substituted with an alkyl group having 1 to 6 carbon atoms), such as a methylcyclohexyl group, a dimethylcyclohexyl group, an ethylcyclohexyl group, a diethylcyclohexyl group, a propylcyclohexyl group, an isopropylcyclohexyl group, a 1-methyl-propylcyclohexyl group, a butylcyclohexyl group, a pentylcyclohexyl group, a pentyl-methylcyclohe
  • Examples of monovalent unsaturated alicyclic hydrocarbon groups include cycloalkenyl groups, such as a cyclohexenyl group, a cycloheptenyl group, and a cyclooctenyl group; and cycloalkenyl groups substituted with an alkyl group having 1 to 6 carbon atoms (preferably cyclohexenyl groups substituted with an alkyl group having 1 to 6 carbon atoms), such as a methylcyclohexenyl group, a dimethylcyclohexenyl group, an ethylcyclohexenyl group, a diethylcyclohexenyl group, and a propylcyclohexenyl group.
  • cycloalkenyl groups such as a cyclohexenyl group, a cycloheptenyl group, and a cyclooctenyl group
  • Examples of monovalent aromatic hydrocarbon groups include a phenyl group, a biphenyl group, a terphenyl group, a naphthyl group, a diphenylmethyl group, a diphenylethyl group, a diphenylpropyl group, a methylphenyl group, a dimethylphenyl group, an ethylphenyl group, and a propylphenyl group.
  • Examples of the divalent aromatic hydrocarbon group that can be selected as R 3 include a phenylene group, a diphenylmethylene group, a diphenylethylene group, a diphenylpropylene group, a methylphenylene group, a dimethylphenylene group, and an ethylphenylene group.
  • a phenylene group, a diphenylmethylene group, a diphenylethylene group, or a diphenylpropylene group is preferred, and a diphenylmethylene group is more preferred.
  • the content of component (B) is preferably 1 to 40% by mass, more preferably 2 to 30% by mass, still more preferably 4 to 25% by mass, and even still more preferably 6 to 20% by mass, based on the whole amount (100% by mass) of the grease composition.
  • component (B) When the content of component (B) is 1% by mass or more, it is easy to adjust the worked penetration of the resulting grease composition to a suitable range.
  • component (B) when the content of component (B) is 40% by mass or less, the resulting grease composition does not become too hard, and it is possible to suppress an adverse effect such as seizure of a portion to be lubricated, such as a bearing, a sliding portion, or a joint portion of the device, to the member, which may be caused by poor lubrication.
  • the urea-based thickener (B) can be usually obtained by reacting an isocyanate compound with a monoamine.
  • the reaction is preferably performed by adding a solution ⁇ obtained by dissolving a monoamine in the base oil (A) to a heated solution ⁇ obtained by dissolving the isocyanate compound in the base oil (A).
  • a diisocyanate having a group corresponding to a divalent aromatic hydrocarbon group represented by R 3 in the general formula (b1) is used as an isocyanate compound, and an amine having a group corresponding to a monovalent hydrocarbon group represented by R 1 and R 2 is used as a monoamine, thus synthesizing a desired urea-based thickener (B) according to the above-described method.
  • component (B) In order to satisfy Requirements (I) and (II), from the viewpoint of dispersing the urea-based thickener (B) in the grease composition, it is preferable to produce component (B) by using a grease manufacturing apparatus as shown in the following [1].
  • Fig. 1 is a schematic cross-sectional view of the grease manufacturing apparatus according to [1] that can be used in one embodiment of the present invention.
  • a grease manufacturing apparatus 1 shown in Fig. 1 includes a container body 2 for introducing a grease raw material into the inside thereof, and a rotor 3 having a rotation axis 12 on a central axis line of an inner periphery of the container body 2 and rotating around the rotation axis 12 as a center axis.
  • the rotor 3 rotates at high speed around the rotation axis 12 as a center axis to apply a high shearing force to a grease raw material inside the container body 2.
  • the grease containing the urea-based thickener (B) is produced.
  • the container body 2 is preferably partitioned from an upper portion to an introduction portion 4, a retention portion 5, a first inner peripheral surface 6, a second inner peripheral surface 7, and a discharge portion 8.
  • the container body 2 has an inner peripheral surface forming such a truncated cone shape that an inner diameter thereof gradually increases from the introduction portion 4 toward the discharge portion 8.
  • the retention portion 5 is disposed in a lower portion of the introduction portion 4, and is a space for temporarily retaining the grease raw material introduced from the introduction portion 4.
  • grease adhering to the inner peripheral surface of the retention portion 5 forms a large lump, so that it is preferable to transport the grease to the first inner peripheral surface 6 in the downstream side in a short time. Further, it is preferable to directly transport to the first inner peripheral surface 6 without passing through the retention portion 5.
  • the first inner peripheral surface 6 is disposed at a lower portion adjacent to the retention portion 5, and the second inner peripheral surface 7 is disposed at a lower portion adjacent to the first inner peripheral surface 6.
  • the discharge portion 8 serving as the other end of the container body 2 is a part for discharging grease agitated by the first inner peripheral surface 6 and the second inner peripheral surface 7, and includes a discharge port 11 for discharging grease.
  • the discharge port 11 is formed in a horizontal direction orthogonal to the rotation axis 12. As a result, grease is discharged from the discharge port 11 in the horizontal direction.
  • the rotor 3 is rotatably provided on the center axis line of the peripheral surface of the container body 2, which has a truncated cone shape, as a rotation axis 12, and rotates counterclockwise when the container body 2 is viewed from the upper portion to the lower portion as shown in Fig. 1 .
  • the rotor 3 has an outer peripheral surface that expands in accordance with the enlargement of the inner diameter of the truncated cone of the container body 2, and the outer peripheral surface of the rotor 3 and the inner peripheral surface of the truncated cone of the container body 2 are maintained at a constant interval.
  • a first concave-convex portion 13 of the rotor in which concave and convex are alternately provided along the surface of the rotor 3 is provided.
  • the first concave-convex portion 13 of the rotor is inclined to the rotation axis 12 of the rotor 3 from the introduction portion 4 toward the discharge portion 8, and has the feeding ability from the introduction portion 4 to the discharge portion 8. That is, the first concave-convex portion 13 of the rotor is inclined in the direction in which the solution is pushed toward the downstream side when the rotor 3 rotates in the direction shown in Fig. 1 .
  • the step difference between a concave portion 13A and a convex portion 13B of the first concave-convex portion 13 of the rotor is preferably 0.3 to 30, more preferably 0.5 to 15, and still more preferably 2 to 7, when the diameter of the concave portion 13A on the outer peripheral surface of the rotor 3 is 100.
  • the number of convex portions 13B of the first concave-convex portion 13 of the rotor in the circumferential direction is preferably 2 to 1000, more preferably 6 to 500, and still more preferably 12 to 200.
  • the ratio of the width of the convex portion 13B to the width of the concave portion 13A of the first concave-convex portion 13 of the rotor [the width of the convex portion/the width of the concave portion] in the cross section orthogonal to the rotation axis 12 of the rotor 3 is preferably 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2.
  • the inclination angle of the first concave-convex portion 13 of the rotor with respect to the rotation axis 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and still more preferably 5 to 20 degrees.
  • the first inner peripheral surface 6 of the container body 2 is provided with the first concave-convex portion 9 formed with a plurality of concave and convex along the inner peripheral surface thereof.
  • the concave and convex of the first concave-convex portion 9 on the container side are inclined in the opposite direction to the first concave-convex portion 13 of the rotor.
  • the plurality of concave and convex of the first concave-convex portion 9 on the container side be inclined in the direction in which the solution is pushed toward the downstream side when the rotation axis 12 of the rotor 3 rotates in the direction shown in Fig. 1 .
  • the stirring capacity and the discharge capacity are further enhanced by the first concave-convex portion 9 having a plurality of concave and convex provided on the first inner peripheral surface 6 of the container body 2.
  • the depth of the concave and convex of the first concave-convex portion 9 on the container side is preferably 0.2 to 30, more preferably 0.5 to 15, and still more preferably 1 to 5, when the inner diameter (diameter) of the container is set to 100.
  • the number of concave and convex of the first concave-convex portion 9 on the container side is preferably 2 to 1000, more preferably 6 to 500, and still more preferably 12 to 200.
  • the ratio of the width of the concave portion to the width of the convex portion between grooves in the concave and convex of the first concave-convex portion 9 on the container side is preferably 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2 or less.
  • the inclination angle of the concave and convex of the first concave-convex portion 9 on the container side with respect to the rotation axis 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and still more preferably 5 to 20 degrees.
  • the first inner peripheral surface 6 can be made to function as a high shearing portion for imparting high shearing force to the grease raw material or grease, but the first concave-convex portion 9 does not necessarily have to be provided.
  • a second concave-convex portion 14 of a rotor having concave and convex alternately provided along the surface of the rotor 3 is provided on the outer peripheral surface of the lower part of the first concave-convex portion 13 of the rotor.
  • the second concave-convex portion 14 of the rotor is inclined with respect to the rotation axis 12 of the rotor 3, and has a feeding suppression ability to push the solution back toward the upstream side from the introduction portion 4 toward the discharge portion 8.
  • the step of the second concave-convex portion 14 of the rotor is preferably 0.3 to 30, more preferably 0.5 to 15, and still more preferably 2 to 7, when the diameter of the concave portion of the outer peripheral surface of the rotor 3 is set to 100.
  • the number of convex portions of the second concave-convex portion 14 of the rotor in the circumferential direction is preferably 2 to 1000, more preferably 6 to 500, and still more preferably 12 to 200.
  • the ratio of the width of the convex portion to the width of the concave portion of the second concave-convex portion 14 of the rotor in a cross section orthogonal to the rotation axis of the rotor 3 is preferably 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2.
  • the inclination angle of the second concave-convex portion 14 of the rotor with respect to the rotation axis 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and still more preferably 5 to 20 degrees.
  • the second inner peripheral surface 7 of the container body 2 is provided with the second concave-convex portion 10 formed with a plurality of concave and convex adjacent to the lower portion of the concave and convex in the first concave-convex portion 9 on the container side.
  • the plurality of concave and convex of the second concave-convex portion 10 on the container side are formed on the inner peripheral surface of the container body 2, and that the concave and convex are inclined in opposite directions to the inclination direction of the second concave-convex portion 14 of the rotor.
  • the plurality of concave and convex of the second concave-convex portion 10 on the container side are inclined in the direction in which the solution is pushed back toward the upstream side when the rotation axis 12 of the rotor 3 rotates in the direction shown in Fig. 1 .
  • the stirring capacity is further enhanced by the concave and convex of the second concave-convex portion 10 provided on the second inner peripheral surface 7 of the container body 2.
  • the second inner peripheral surface 7 of the container body can function as a high shearing portion which imparts a high shearing force to the grease raw material or grease.
  • the depth of the concave portion of the second concave-convex portion 10 on the container side is preferably 0.2 to 30, more preferably 0.5 to 15, and still more preferably 1 to 5, when the inner diameter (diameter) of the container is set to 100.
  • the number of concave portions of the second concave-convex portion 10 on the container side is preferably 2 to 1000, more preferably 6 to 500, and still more preferably 12 to 200.
  • the ratio of the width of the convex portion of the concave and convex of the second concave-convex portion 10 on the container side to the width of the concave portion in the cross section orthogonal to the rotation axis 12 of the rotor 3 [width of the convex portion / width of the concave portion] is preferably 0.01 to 100, more preferably 0.1 to 10, and still more preferably 0.5 to 2 or less.
  • the inclination angle of the second concave-convex portion 10 on the container side with respect to the rotation axis 12 is preferably 2 to 85 degrees, more preferably 3 to 45 degrees, and still more preferably 5 to 20 degrees.
  • the ratio of the length of the first concave-convex portion 9 on the container side to the length of the second concave-convex portion 10 on the container side [length of the first concave-convex portion / length of the second concave-convex portion] is preferably 2/1 to 20/1.
  • Fig. 2 is a horizontal cross-sectional view of the first concave-convex portion 9 on the container side of the grease manufacturing apparatus 1.
  • a plurality of scrapers 15 each having a tip protruding toward the inner peripheral surface side of the container body 2 are provided more than the tip end in the projecting direction of the convex portion 13B of the first concave-convex portion 13.
  • the second concave-convex portion 14 is also provided with a plurality of scrapers in which the tip of the convex portion protrudes toward the inner peripheral surface side of the container body 2, similarly to the first concave-convex portion 13.
  • the scraper 15 scrapes off the grease adhering to the inner peripheral surface of the first concave-convex portion 9 on the container side and the second concave-convex portion 10 on the container side.
  • the ratio [R2/R1] of the radius (R2) of the tip of the scraper 15 to the radius (R1) of the tip of the convex portion 13B is preferably more than 1.005 and less than 2.0.
  • the number of scrapers 15 is preferably 2 to 500, more preferably 2 to 50, and still more preferably 2 to 10.
  • the scraper 15 is provided, but may not be provided, or may be provided intermittently.
  • the solution ⁇ and the solution ⁇ which are the aforementioned grease raw materials are introduced respectively from the solution introducing pipes 4A and 4B of the introduction portion 4 of the container body 2, and the rotor 3 is rotated at high speed to produce the grease containing the urea-based thickener (B).
  • the urea-based thickener (B) can be dispersed in the grease composition so as to satisfy the above Requirements (I) and (II) even if an additive containing an antioxidant (C) and a rust inhibitor (D) is blended.
  • the shear rate applied to the grease raw material is preferably 10 2 s -1 or more, more preferably 10 3 s -1 or more, still more preferably 10 4 s -1 or more, and is usually 10 7 s -1 or less.
  • the ratio of the maximum shear rate (Max) to the minimum shear rate (Min) in the shearing at the time of high-speed rotation of the rotor 3 is preferably 100 or less, more preferably 50 or less, and still more preferably 10 or less.
  • the shear rate to the mixed solution is as uniform as possible, the dispersion state of the thickener and its precursor is improved and a uniform grease structure is obtained.
  • Maximum shear rate Min linear velocity at the tip of the convex portion 13 B of the first concave ⁇ convex portion 13 of the rotor / a gap A 1 between the tip end of the convex portion 13 B of the first concave ⁇ convex portion 13 of the rotor and the convex portion of the first concave ⁇ convex portion 9 on the container side of the first concave ⁇ convex portion 6 .
  • Minimum shear rate Min linear velocity of the convex portion 13 A of the first concave ⁇ convex portion 13 of the rotor / a gap A2 between the convex portion 13 A of the first concave ⁇ convex portion 13 of the rotor and the concave portion of the first concave ⁇ convex portion 9 on the container side of the first concave ⁇ convex portion 6 .
  • the gap A1 and the gap A2 are as shown in Fig. 2 .
  • the grease manufacturing apparatus 1 is provided with the scraper 15, grease adhering to the inner peripheral surface of the container body 2 can be scraped off, so that the generation of the lumps during kneading can be prevented, and the grease in which the urea-based thickener (B) is highly dispersed can be continuously produced in a short time.
  • the scraper 15 scrapes off the grease adhered thereto, it is possible to prevent the retained grease from becoming a resistance to rotation of the rotor 3, so that the rotational torque of the rotor 3 can be reduced, and the power consumption of the drive source can be reduced, thereby making it possible to continuously manufacture the grease efficiently.
  • the centrifugal force has an effect of discharging the grease or grease raw material in the downstream direction, and the rotation torque of the rotor 3 can be reduced to continuously manufacture the grease.
  • the first concave-convex portion 13 of the rotor is provided on an outer peripheral surface of the rotor 3, the first concave-convex portion 13 of the rotor is inclined with respect to the rotation axis 12 of the rotor 3, and a feeding ability from the introduction portion 4 to the discharge portion 8 is provided, and the second concave-convex portion 14 of the rotor is inclined with respect to the rotation axis 12 of the rotor 3, and a feeding suppression ability from the introduction portion 4 to the discharge portion 8 is provided, a high shear force can be applied to the solution, and the urea-based thickener (B) can be dispersed in the grease composition so as to satisfy the above-mentioned Requirements (I) and (II) even after blending the additive.
  • the first concave-convex portion 9 on the container side is formed on the first inner peripheral surface 6 of the container body and is inclined in the opposite direction to the first concave-convex portion 13 of the rotor, in addition to the effect of the first concave-convex portion 13 of the rotor, sufficient stirring of grease raw material can be carried out while extruding grease or grease raw material in the downstream direction, and the urea-based thickener (B) can be dispersed in the grease composition so as to satisfy the above Requirements (I) and (II) even after blending the additive.
  • the grease raw material can be prevented from flowing out from the first inner peripheral surface 6 of the container body more than necessary, so that the urea-based thickener (B) can be dispersed in the grease composition so as to satisfy Requirements (I) and (II) even after blending the additive by giving high shear force to the solution to highly disperse the grease raw material.
  • the antioxidant (C) contained in the grease composition of the present invention may be a compound capable of imparting antioxidant performance, and preferably contains one or more kinds selected from an amine antioxidant (C1) and a phenol-based antioxidant (C2).
  • the antioxidant (C) used in one embodiment of the present invention may be used alone or in combination of two or more thereof.
  • amine antioxidant (C1) a compound having an amino group may be used, and a diphenylamine compound and a naphthylamine compound are preferred.
  • diphenylamine compound examples include monoalkyldiphenylamine compounds having one alkyl group having 1 to 30 carbon atoms (preferably 4 to 30, more preferably 8 to 30), such as monooctyl diphenylamine, and monononyl diphenylamine; dialkyldiphenylamine compounds having two alkyl groups having 1 to 30 carbon atoms (preferably 4 to 30, more preferably 8 to 30), such as 4,4'-dibutyldiphenylamine, 4,4'-dipentyldiphenylamine, 4,4'-dihexyldiphenylamine, 4,4'-diheptyldiphenylamine, 4,4'-dioctyldiphenylamine, and 4,4'-dinonyldiphenylamine; polyalkyldiphenylamine compounds having 3 or more alkyl groups having 1 to 30 carbon atoms (preferably 4 to 30 and more preferably 8 to 30), such as tetrabutyldiphenylamine
  • naphthylamine compound examples include 1-naphthylamine, phenyl-1-naphthylamine, butylphenyl-1-naphthylamine, pentylphenyl-1-naphthylamine, hexylphenyl-1-naphthylamine, heptylphenyl-1-naphthylamine, octylphenyl-1-naphthylamine, nonylphenyl-1-naphthylamine, decylphenyl-1-naphthylamine, and dodecylphenyl-1-naphthylamine.
  • a compound represented by the following general formula (c1-1) is preferable.
  • a compound represented by the following general formula (c1-2) or a compound represented by the following general formula (c1-3) is preferable.
  • R 11 to R 18 are each independently an alkyl group having 1 to 20 carbon atoms (preferably 4 to 18, more preferably 6 to 16, and still more preferably 8 to 14).
  • the alkyl group include the same alkyl groups as those having 1 to 20 carbon atoms among the alkyl groups that the alkylbenzene (B) may have.
  • n1, n2, n3, and n6 are each independently an integer of 0 to 5, preferably an integer of 0 to 3, more preferably an integer of 0 to 1, and still more preferably 1.
  • m4 and m7 are each independently an integer of 0 to 3, preferably an integer of 0 to 1, and more preferably 0.
  • p5 and p8 are each independently an integer of 0 to 4, preferably an integer of 0 to 2, more preferably an integer of 0 to 1, and still more preferably 0.
  • phenol-based antioxidant (C2) examples include monocyclic phenol compounds such as 2,6-di-tert-butyl-4-methylphenol, 2,6-di-tert-butyl-4-ethylphenol, 2,4,6-tri-tert-butylphenol, 2,6-di-tert-butyl-4-hydroxymethylphenol, 2,6-di-tert-butylphenol, 2,4-dimethyl-6-tert-butylphenol, 2,6-di-tert-butyl-4-(N,N-dimethylaminomethyl)phenol, 2,6-di-tert-amyl-4-methylphenol, and n-octadecyl-3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, and polycyclic phenol compounds such as 4,4'-methylenebis (2,6-di-tert-butylphenol), 4,4'-isopropylidenebis(2,6-di-tert)
  • phenol-based antioxidants (D2) may be used alone or in combination of two or more.
  • the phenol-based antioxidant (C2) may be a compound having a phenol structure, and may be a monocyclic phenol compound or a polycyclic phenol compound.
  • Examples of the monocyclic phenol compound include, for example, 2,6-di-tert-butyl-4-methylphenol, 2,6-di-tert-butyl-4-ethylphenol, 2,4,6-tri-tert-butylphenol, 2,6-di-tert-butyl-4-hydroxymethylphenol, 2,6-di-tert-butylphenol, 2,4-dimethyl-6-tert-butylphenol, 2,6-di-tert-butyl-4-(N,N-dimethylaminomethyl)phenol, 2,6-di-tert-amyl-4-methylphenol, and benzenepropanoic acid 3,5-bis(1,1-dimethylethyl)-4-hydroxyalkyl ester.
  • polycyclic phenol compound examples include, for example, 4,4'-methylenebis(2,6-di-tert-butylphenol), 4,4'-isopropylidenebis(2,6-di-tert-butylphenol), 2,2'-methylenebis(4-methyl-6-tert-butylphenol), 4,4'-bis(2,6-di-tert-butylphenol), 4,4'-bis(2-methyl-6-tert-butylphenol), 2,2'-methylenebis(4-ethyl-6-tert-butylphenol), and 4,4'-butylidenebis(3-methyl-6-tert-butylphenol).
  • the content of the component (C) is preferably 0.01 to 15% by mass, more preferably 0.05 to 10% by mass, still more preferably 0.10 to 7% by mass, and even still more preferably 0.50 to 4% by mass based on the whole amount (100% by mass) of the grease composition.
  • the rust inhibitor (D) contained in the grease composition of the present invention may be any compound capable of imparting rust preventive performance, and examples thereof include zinc stearate, a carboxylic acid type rust inhibitor, a succinic acid derivative, a thiadiazole and derivatives thereof, benzotriazole and derivatives thereof, sodium nitrite, petroleum sulfonate, sorbitan monooleate, fatty acid soap, and amine compounds.
  • rust inhibitors (D) may be used alone or in combination of two or more thereof.
  • rust inhibitor (D) used in one embodiment of the present invention a carboxylic acid rust inhibitor is preferable.
  • the carboxylic acid rust inhibitor is more preferably a succinic acid ester, and more preferably an alkenyl succinic acid polyhydric alcohol ester.
  • the alkenyl succinic acid polyhydric alcohol ester is an ester of an alkenyl succinic acid and a polyhydric alcohol.
  • the alkenyl group of alkenyl succinic acid is preferably an alkenyl group having 12 to 20 carbon atoms, and specific examples include dodecenyl, hexadecenyl, octadecenyl, and isooctadecenyl.
  • polyhydric alcohol examples include saturated dihydric alcohols having 1 to 6 carbon atoms such as ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, and structural isomers thereof; trivalent or higher saturated polyhydric alcohols such as trimethylolpropane, trimethylolbutane, glycerin, pentaerythritol, and dipentaerythritol.
  • the content of component (D) is preferably 0.01 to 5% by mass, more preferably 0.03 to 3% by mass, still more preferably 0.05 to 2% by mass, and even still more preferably 0.10 to 1% by mass based on the whole amount (100% by mass) of the grease composition.
  • the grease composition according to one embodiment of the present invention may contain, besides components (A) to (D), other additives, which are those blended in general grease, within a range that does not impair the effects of the present invention.
  • Such additives include, for example, extreme pressure agents, viscosity improvers, solid lubricants, cleaning dispersants, corrosion inhibitors, metal deactivators, and the like.
  • additives may be used alone or in combination of two or more thereof.
  • extreme pressure agents include thiocarbamic acids such as zinc dialkyldithiophosphate, molybdenum dialkyldithiophosphate, ashless dithiocarbamate, and zinc dithiocarbamate; sulfur compounds such as sulfurized fats and oils, sulfurized olefins, polysulfide, thiophosphoric acids, thioterpenes, and dialkylthiopropionate; phosphate esters such as tricresyl phosphate; and phosphite esters such as triphenyl phosphite.
  • thiocarbamic acids such as zinc dialkyldithiophosphate, molybdenum dialkyldithiophosphate, ashless dithiocarbamate, and zinc dithiocarbamate
  • sulfur compounds such as sulfurized fats and oils, sulfurized olefins, polysulfide, thiophosphoric acids, thioterpenes, and dialkylthiopropionat
  • viscosity improvers examples include polymethacrylate (PMA), olefin copolymer (OCP), polyalkylstyrene (PAS), and styrene-diene copolymer (SCP).
  • PMA polymethacrylate
  • OCP olefin copolymer
  • PAS polyalkylstyrene
  • SCP styrene-diene copolymer
  • solid lubricants examples include polyimide, PTFE, graphite, metal oxide, boron nitride, melamine cyanurate (MCA), and molybdenum disulfide.
  • cleaning dispersants include ashless dispersants such as succinimide and boron succinimide.
  • corrosion inhibitors examples include benzotriazole compounds and thiazole compounds.
  • metal deactivators examples include benzotriazole compounds.
  • the contents of the other additives are each independently usually 0 to 10% by mass, preferably 0 to 7% by mass, more preferably 0 to 5% by mass, and still more preferably 0 to 2% by mass based on the whole amount (100% by mass) of the grease composition
  • the heating temperature of the grease containing the base oil (A) and the urea-based thickener (B) in blending the additive and in stirring after the blending is preferably 80 to 200°C, more preferably 90 to 180°C, still more preferably 100 to 160°C, and even still more preferably 110 to 140°C.
  • the worked penetration of the grease composition according to one embodiment of the present invention at 25°C is preferably 180 to 300, more preferably 200 to 290, still more preferably 220 to 285, and even still more preferably 240 to 280.
  • the worked penetration of the grease composition means a value measured at 25°C in accordance with the ASTM D217 test method.
  • the dropping point of the grease composition according to one embodiment of the present invention is preferably 240°C or higher, more preferably 250°C or higher, still more preferably 255°C or higher, and even still more preferably 260°C or higher.
  • the oxidation stability of the prepared grease composition was measured in accordance with JIS K2220 12:2013.
  • Fig. 4 is a particle size distribution curve obtained by measuring the particle size of particles containing a urea-based thickener (B) in the grease composition produced in Example 1 on a volume basis with light scattering.
  • the particle size r 1 of the peak P 1 indicating the maximum frequency y 1 was 0.6 ⁇ m
  • the half width x 1 of the peak P 1 was 0.6 ⁇ m
  • Requirements (I) and (II) were satisfied.
  • Fig. 5 is a particle size distribution curve obtained by measuring particle size of particles containing the urea-based thickener (B) in the grease composition produced in Comparative Example 1 on a volume basis with light scattering.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
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CN117295807A (zh) * 2021-03-31 2023-12-26 出光兴产株式会社 润滑脂组合物

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