WO2012115141A1 - Grease composition - Google Patents

Grease composition Download PDF

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Publication number
WO2012115141A1
WO2012115141A1 PCT/JP2012/054256 JP2012054256W WO2012115141A1 WO 2012115141 A1 WO2012115141 A1 WO 2012115141A1 JP 2012054256 W JP2012054256 W JP 2012054256W WO 2012115141 A1 WO2012115141 A1 WO 2012115141A1
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Prior art keywords
grease composition
thickener
cyclohexyl
formula
group
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PCT/JP2012/054256
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French (fr)
Japanese (ja)
Inventor
山本 正道
雄太 佐藤
Original Assignee
協同油脂株式会社
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Publication date
Application filed by 協同油脂株式会社 filed Critical 協同油脂株式会社
Priority to DE112012000940T priority Critical patent/DE112012000940T5/en
Priority to KR1020137020084A priority patent/KR20130118936A/en
Priority to US13/983,665 priority patent/US20130310292A1/en
Priority to CN201280009920.9A priority patent/CN103415603B/en
Publication of WO2012115141A1 publication Critical patent/WO2012115141A1/en

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M115/00Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • C10M169/02Mixtures of base-materials and thickeners
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/02Well-defined aliphatic compounds
    • C10M2203/0206Well-defined aliphatic compounds used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028Organic 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
    • C10M2205/0285Organic 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/282Esters of (cyclo)aliphatic oolycarboxylic acids
    • C10M2207/2825Esters of (cyclo)aliphatic oolycarboxylic acids used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
    • C10M2207/2835Esters of polyhydroxy compounds used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10Amides of carbonic or haloformic acids
    • C10M2215/102Ureas; Semicarbazides; Allophanates
    • C10M2215/1026Ureas; Semicarbazides; Allophanates used as thickening material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02Pour-point; Viscosity index
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/04Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16CSHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/30Parts of ball or roller bearings
    • F16C33/66Special parts or details in view of lubrication
    • F16C33/6603Special parts or details in view of lubrication with grease as lubricant
    • F16C33/6633Grease properties or compositions, e.g. rheological properties

Definitions

  • the present invention relates to a grease composition that can be used for lubricating various machine parts such as rolling bearings, gears, ball screws, linear motion bearings, cams, and joints.
  • the sealing device Since grease can be lubricated without lubrication for a long period of time, the sealing device is simple, the required amount is small, and there is little fouling due to leakage. It is used in many machine parts that have a body. However, since grease is a semi-solid lubricant containing a base oil and a thickener, it has a higher apparent viscosity and a higher stirring resistance than a lubricant. In the past, in order to reduce the agitation resistance of grease, it has been a common practice to make the kinematic viscosity of the base oil as low as possible as in the case of lubricating oil.
  • Patent Document 1 proposes a grease composition using a base oil containing a diester oil having a specific structure, and an example describes a diester oil having a kinematic viscosity at 40 ° C. of 20.16 mm 2 / s. Has been. However, if the kinematic viscosity of the base oil of the grease is lowered, the stirring resistance will be reduced. The base oil that can be used is limited because it disappears.
  • the problem to be solved by the present invention is to provide a grease composition having a low stirring resistance.
  • Another object of the present invention is to provide a mechanical component enclosing the grease composition.
  • the present inventors solved this problem by selecting an appropriate thickener. That is, according to the present invention, the following grease composition and machine parts are provided: 1. A thickener, a base oil, the thickener is a diurea compound represented by the following formula (1), and the amount of the thickener in the grease composition is 3 to 20% by mass: Grease composition.
  • R 2 represents a diphenylmethane group.
  • R 1 and R 3 may be the same or different, and represent a cyclohexyl group or a linear or branched alkyl group having 8 to 22 carbon atoms.
  • the ratio of the number of moles of cyclohexyl group to the total number of moles of cyclohexyl group and alkyl group [ ⁇ (number of cyclohexyl groups) / (number of cyclohexyl groups + alkyl group Number) ⁇ ⁇ 100] is 70 to 80 mol%.) 2.
  • a grease composition having a low stirring resistance can be provided.
  • the grease composition of the present invention can suppress the occurrence of oil film breakage without lowering the kinematic viscosity of the base oil, and can satisfy a sufficiently long life.
  • diurea grease As a thickener for grease, diurea grease having a long lubrication life and general versatility is generally used.
  • Such diurea grease is represented by the following formula (1):
  • R 2 represents a diphenylmethane group. 4,4-diphenylmethane is preferred.
  • R 1 and R 3 may be the same or different and each represents a cyclohexyl group or a linear or branched, preferably linear alkyl group having 8 to 22 carbon atoms, preferably 16 to 20 carbon atoms.
  • the ratio of the number of moles of cyclohexyl group to the total number of moles of cyclohexyl group and alkyl group [ ⁇ (number of cyclohexyl groups) / (number of cyclohexyl groups + number of alkyl groups) ) ⁇ ⁇ 100] is 70 to 80 mol%.
  • the amount of the thickener can be reduced.
  • the stirring resistance of the grease can be reduced.
  • the content of the thickener is 3 to 20% by mass, preferably 5 to 15% by mass, based on the mass of the grease composition of the present invention.
  • Metal soaps, benton, and silica gel do not satisfy heat resistance, that is, bearing lubrication life at high temperatures. Fluorine-based thickeners are very expensive, although they are satisfactory in heat resistance, and lack versatility.
  • the type and kinematic viscosity of the base oil in the present invention are not particularly limited.
  • the type and kinematic viscosity of the base oil can be selected as necessary.
  • the kinematic viscosity at 40 ° C. of the base oil contained in the grease used for the rolling bearing is preferably 10 to 200 mm 2 / s, more preferably 15 to 100 mm 2 / s.
  • a base oil may be used individually by 1 type, and may use 2 or more types together.
  • the types of base oils that can be used in the present invention are roughly classified into mineral oils and synthetic oils.
  • synthetic oils include diester oils, ester-based synthetic oils represented by polyol esters, poly- ⁇ -olefins, synthetic hydrocarbon oils represented by polybutene, ether-based synthetic oils represented by alkyl diphenyl ether, and polypropylene glycol.
  • Representative examples include polyglycol-based synthetic oils, silicone-based synthetic oils, and fluorine-based synthetic oils. Of these, synthetic oil is preferred because of its excellent heat resistance. Synthetic hydrocarbon oils and ester synthetic oils are more preferred. When these base oils are included, the stirring resistance at low temperatures can be further reduced.
  • the synthetic hydrocarbon oil is preferably poly- ⁇ -olefin.
  • ester synthetic oil pentaerythritol ester and trimethylolpropane ester are preferable.
  • the grease composition of the present invention can contain any additive as required.
  • antioxidants typified by amines and phenols
  • inorganic passivating agents such as sodium nitrite, sulfonates, succinic acids, amines, rust inhibitors typified by carboxylates, and benzotriazoles.
  • Representative metal corrosion inhibitors, fatty agents such as fatty acids, fatty acid esters and phosphate esters, antiwear and extreme pressure agents such as phosphorus, sulfur and organometallics, metal oxides and disulfides
  • solid lubricants typified by molybdenum. The amount of these components used is usually about 0.1 to 20% by mass, preferably 0.5 to 10% by mass.
  • the penetration of the grease composition of the present invention is adjusted according to the purpose of use, but is preferably 200 to 440. In particular, for bearings, if it is too soft, there is a concern of leakage, so 200 to 350 is preferable.
  • the grease composition of the present invention can be used by being enclosed in various machine parts.
  • various machine parts include rolling bearings, gears, ball screws, linear motion bearings, cams, and joints.
  • various motors for industrial machines various motors for office equipment, various motors for automobiles, rolling bearings used for automobile electrical parts and auxiliary machine parts, windmills, robots, reduction gears and speed increasers for automobiles, etc.
  • ⁇ Test method> ⁇ Agitation resistance (rheometer) The test was performed using a viscoelasticity measuring device manufactured by Anton Paar, Physica MCR301. The test grease was applied between the predetermined plates, and after setting the predetermined distance between the plates, the excess grease that protruded was removed. Then, the shear stress when rotating at the shear rate shown below was read. Test conditions are shown below. Shear rate: 1 to 10 4 s -1 Test temperature: 25 ° C Distance between plates: 0.2mm Plate diameter: 25mm ⁇ Evaluation> An average value of shear stress at a shear rate of 1 to 10 4 s ⁇ 1 was calculated and used as a measurement result. Less than 2000Pa ⁇ ⁇ ⁇ Pass 2000Pa or more ⁇ ⁇ ⁇ Fail

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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)
  • Rolling Contact Bearings (AREA)

Abstract

The present invention provides a grease composition which comprises a thickening agent and a base oil, wherein the thickening agent is a diurea compound represented by formula (1) and the proportion of the thickening agent in the grease composition is 3-20 mass%. (In formula (1), R2 represents a diphenylmethane group. R1 and R3 may be the same or different and each represent a cyclohexyl group or a linear or branched C8-22 alkyl group. In formula (1), the proportion of the number of moles of cyclohexyl groups to the total number of moles of cyclohexyl groups and alkyl groups [{(number of cyclohexyl groups)/((number of cyclohexyl groups)+(number of alkyl groups))}×100] is 70-80 mol%.)

Description

グリース組成物Grease composition
 本発明は、転がり軸受、歯車、ボールネジ、直動軸受、カム又は継ぎ手等の各種機械部品の潤滑に使用できるグリース組成物に関する。 The present invention relates to a grease composition that can be used for lubricating various machine parts such as rolling bearings, gears, ball screws, linear motion bearings, cams, and joints.
 近年、消費エネルギー削減の観点から、自動車を始め、各産業で使用される電気機器や機械部品は、高効率化が求められており、部品の軽量化や構造の改良など、種々の検討がなされている。特に回転体を持つ機械部品は、潤滑剤が攪拌されるため、その抵抗がエネルギーロスに繋がる。したがって、攪拌抵抗の低い潤滑剤が求められている。
 例えばエンジン油やトランスミッション油では、潤滑油の攪拌抵抗を低減するために、低粘度化が提案されている(非特許文献1および2)。しかしながら、これらの対策では、油の低粘度化に起因した油膜切れを起こし、潤滑部表面の損傷が懸念される。
In recent years, from the viewpoint of reducing energy consumption, electrical equipment and machine parts used in various industries including automobiles have been required to be highly efficient, and various studies have been made such as weight reduction of parts and improvement of structure. ing. In particular, the mechanical component having a rotating body stirs the lubricant, so that its resistance leads to energy loss. Therefore, there is a demand for a lubricant with low stirring resistance.
For example, in engine oil and transmission oil, low viscosity has been proposed in order to reduce the stirring resistance of lubricating oil (Non-patent Documents 1 and 2). However, these countermeasures cause oil film breakage due to low viscosity of the oil, and there is a concern about damage to the surface of the lubrication part.
 グリースは長期間、無給脂でも潤滑できることや、密封装置が単純であること、必要量が少ないこと、漏れによる汚損が少ないことなど、潤滑油と比較して優れている点があることから、回転体を持つ多くの機械部品に使用されている。しかしながら、グリースは、基油と増ちょう剤を含む半固体状の潤滑剤であるため、潤滑油と比較し、見掛け粘度が高く、攪拌抵抗が大きい。
 これまで、グリースの攪拌抵抗を低減するために、潤滑油の場合と同様に、基油の動粘度をできるだけ低くすることが常套手段とされてきた。例えば特許文献1では、特定構造であるジエステル油を含有する基油を用いたグリース組成物が提案されており、実施例には40℃における動粘度が20.16mm2/sのジエステル油が記載されている。
 しかし、グリースの基油の動粘度を下げると攪拌抵抗は低減するものの、潤滑油について述べたのと同様に、油膜切れが発生し、充分な寿命、例えば、はく離寿命、焼付き寿命が満足できなくなるため、使用可能な基油は限定されている。
Since grease can be lubricated without lubrication for a long period of time, the sealing device is simple, the required amount is small, and there is little fouling due to leakage. It is used in many machine parts that have a body. However, since grease is a semi-solid lubricant containing a base oil and a thickener, it has a higher apparent viscosity and a higher stirring resistance than a lubricant.
In the past, in order to reduce the agitation resistance of grease, it has been a common practice to make the kinematic viscosity of the base oil as low as possible as in the case of lubricating oil. For example, Patent Document 1 proposes a grease composition using a base oil containing a diester oil having a specific structure, and an example describes a diester oil having a kinematic viscosity at 40 ° C. of 20.16 mm 2 / s. Has been.
However, if the kinematic viscosity of the base oil of the grease is lowered, the stirring resistance will be reduced. The base oil that can be used is limited because it disappears.
特開2009-132754公報JP 2009-132754 A
 本発明が解決しようとする課題は、攪拌抵抗を低くしたグリース組成物を提供することである。
 本発明はまた、前記グリース組成物を封入した機械部品を提供することを課題とする。
The problem to be solved by the present invention is to provide a grease composition having a low stirring resistance.
Another object of the present invention is to provide a mechanical component enclosing the grease composition.
 本発明者らは、上記課題に対し、適切な増ちょう剤を選定することでこれを解決した。
すなわち、本発明により、以下のグリース組成物及び機械部品を提供する:
1. 増ちょう剤と、基油とを含み、前記増ちょう剤が下記式(1)で示されるジウレア化合物であり、かつグリース組成物中の前記増ちょう剤量の割合が3~20質量%であるグリース組成物。
The present inventors solved this problem by selecting an appropriate thickener.
That is, according to the present invention, the following grease composition and machine parts are provided:
1. A thickener, a base oil, the thickener is a diurea compound represented by the following formula (1), and the amount of the thickener in the grease composition is 3 to 20% by mass: Grease composition.
Figure JPOXMLDOC01-appb-C000002
Figure JPOXMLDOC01-appb-C000002
(式(1)中、R2は、ジフェニルメタン基を示す。R1及びR3は、同一でも異なっていてもよく、シクロへキシル基又は炭素数8~22の直鎖又は分岐アルキル基を示す。式(1)中、シクロへキシル基とアルキル基の総モル数に対するシクロへキシル基のモル数の割合[{(シクロへキシル基の数)/(シクロへキシル基の数+アルキル基の数)}×100]は70~80モル%である。)
2. 増ちょう剤が、式(1)中、アルキル基が炭素数16~20の直鎖アルキル基であるジウレア化合物である、前記1項記載のグリース組成物。
3. 転がり軸受、歯車、ボールネジ、直動軸受、カム又は継ぎ手に使用される、前記1又は2項記載のグリース組成物。
4. 前記1~3のいずれか1項記載のグリース組成物を封入した機械部品。
(In formula (1), R 2 represents a diphenylmethane group. R 1 and R 3 may be the same or different, and represent a cyclohexyl group or a linear or branched alkyl group having 8 to 22 carbon atoms. In the formula (1), the ratio of the number of moles of cyclohexyl group to the total number of moles of cyclohexyl group and alkyl group [{(number of cyclohexyl groups) / (number of cyclohexyl groups + alkyl group Number)} × 100] is 70 to 80 mol%.)
2. 2. The grease composition as described in 1 above, wherein the thickener is a diurea compound in which the alkyl group is a linear alkyl group having 16 to 20 carbon atoms in the formula (1).
3. 3. The grease composition according to the above 1 or 2, which is used for rolling bearings, gears, ball screws, linear motion bearings, cams or joints.
4). A machine part in which the grease composition according to any one of 1 to 3 is encapsulated.
 本発明により、攪拌抵抗を低くしたグリース組成物を提供することができる。本発明のグリース組成物は、基油の動粘度を下げることなく、油膜切れの発生を抑制し、充分に長い寿命を満足できる。 According to the present invention, a grease composition having a low stirring resistance can be provided. The grease composition of the present invention can suppress the occurrence of oil film breakage without lowering the kinematic viscosity of the base oil, and can satisfy a sufficiently long life.
〔増ちょう剤〕
 グリースの増ちょう剤としては、一般的に、長い潤滑寿命を示し、且つ汎用性のあるジウレアグリースが多く使用されている。本発明では、脂環式アミンと脂肪族アミンとを特定モル比で配合することにより製造されるジウレアグリースを選定した。かかるジウレアグリースは下記式(1)で表される:
[Thickener]
As a thickener for grease, diurea grease having a long lubrication life and general versatility is generally used. In this invention, the diurea grease manufactured by mix | blending an alicyclic amine and an aliphatic amine by specific molar ratio was selected. Such diurea grease is represented by the following formula (1):
Figure JPOXMLDOC01-appb-C000003
 式(1)中、R2は、ジフェニルメタン基を示す。4,4-ジフェニルメタンが好ましい。R1及びR3は、同一でも異なっていてもよく、シクロへキシル基又は炭素数8~22、好ましくは炭素数16~20の直鎖又は分岐、好ましくは直鎖アルキル基を示す。式(1)中、シクロへキシル基とアルキル基の総モル数に対するシクロへキシル基のモル数の割合[{(シクロへキシル基の数)/(シクロへキシル基の数+アルキル基の数)}×100]は、70~80モル%である。
Figure JPOXMLDOC01-appb-C000003
In formula (1), R 2 represents a diphenylmethane group. 4,4-diphenylmethane is preferred. R 1 and R 3 may be the same or different and each represents a cyclohexyl group or a linear or branched, preferably linear alkyl group having 8 to 22 carbon atoms, preferably 16 to 20 carbon atoms. In formula (1), the ratio of the number of moles of cyclohexyl group to the total number of moles of cyclohexyl group and alkyl group [{(number of cyclohexyl groups) / (number of cyclohexyl groups + number of alkyl groups) )} × 100] is 70 to 80 mol%.
 前記増ちょう剤を使用することにより、増ちょう剤の量を低減することができる。前記増ちょう剤を基油に特定量含ませることにより、グリースの攪拌抵抗を低減することができる。具体的には、増ちょう剤の含有量は、本発明のグリース組成物の質量に対して、3~20質量%、好ましくは5~15質量%である。
 なお、金属石けん類、ベントン、シリカゲルは、耐熱性、すなわち高温下での軸受潤滑寿命を満足するものではない。またフッ素系増ちょう剤は、耐熱性は満足するものの非常に高価であり、汎用性に欠ける。
By using the thickener, the amount of the thickener can be reduced. By adding a specific amount of the thickener to the base oil, the stirring resistance of the grease can be reduced. Specifically, the content of the thickener is 3 to 20% by mass, preferably 5 to 15% by mass, based on the mass of the grease composition of the present invention.
Metal soaps, benton, and silica gel do not satisfy heat resistance, that is, bearing lubrication life at high temperatures. Fluorine-based thickeners are very expensive, although they are satisfactory in heat resistance, and lack versatility.
〔基油〕
 本発明における基油の種類や動粘度は特に限定されない。必要に応じて基油の種類や動粘度を選定することができる。ただし、転がり軸受用として使用するグリースに含ませる基油の40℃における動粘度としては、好ましくは10~200mm2/s、より好ましくは15~100mm2/sである。基油は、一種を単独で使用しても良く、2種以上を併用しても良い。
 本発明において使用可能な基油の種類としては、大別して鉱物油、合成油がある。合成油の例としてはジエステル油、ポリオールエステルに代表されるエステル系合成油、ポリ-α-オレフィン、ポリブテンに代表される合成炭化水素油、アルキルジフェニルエーテルに代表されるエーテル系合成油、ポリプロピレングリコールに代表されるポリグリコール系合成油、シリコーン系合成油、フッ素系合成油が挙げられる。このうち、耐熱性に優れるため合成油が好ましい。合成炭化水素油及びエステル系合成油がより好ましい。これら基油を含ませると、低温での撹拌抵抗をより低くすることができる。合成炭化水素油としてはポリ-α-オレフィンが好ましい。エステル系合成油としてはペンタエリスリトールエステル、トリメチロールプロパンエステルが好ましい。
[Base oil]
The type and kinematic viscosity of the base oil in the present invention are not particularly limited. The type and kinematic viscosity of the base oil can be selected as necessary. However, the kinematic viscosity at 40 ° C. of the base oil contained in the grease used for the rolling bearing is preferably 10 to 200 mm 2 / s, more preferably 15 to 100 mm 2 / s. A base oil may be used individually by 1 type, and may use 2 or more types together.
The types of base oils that can be used in the present invention are roughly classified into mineral oils and synthetic oils. Examples of synthetic oils include diester oils, ester-based synthetic oils represented by polyol esters, poly-α-olefins, synthetic hydrocarbon oils represented by polybutene, ether-based synthetic oils represented by alkyl diphenyl ether, and polypropylene glycol. Representative examples include polyglycol-based synthetic oils, silicone-based synthetic oils, and fluorine-based synthetic oils. Of these, synthetic oil is preferred because of its excellent heat resistance. Synthetic hydrocarbon oils and ester synthetic oils are more preferred. When these base oils are included, the stirring resistance at low temperatures can be further reduced. The synthetic hydrocarbon oil is preferably poly-α-olefin. As the ester synthetic oil, pentaerythritol ester and trimethylolpropane ester are preferable.
〔添加剤〕
 本発明のグリース組成物は、必要に応じてあらゆる添加剤を含むことができる。例として、アミン系、フェノール系に代表される酸化防止剤、亜硝酸ソーダなどの無機不働態化剤、スルホネート系、コハク酸系、アミン系、カルボン酸塩に代表される錆止め剤、ベンゾトリアゾールに代表される金属腐食防止剤、脂肪酸、脂肪酸エステル、リン酸エステルに代表される油性剤、リン系、硫黄系、有機金属系に代表される耐摩耗剤や極圧剤、酸化金属塩や二硫化モリブデンに代表される固体潤滑剤などが挙げられる。これらの成分の使用量は、通常0.1~20質量%程度、好ましくは0.5~10質量%である。
〔Additive〕
The grease composition of the present invention can contain any additive as required. Examples include antioxidants typified by amines and phenols, inorganic passivating agents such as sodium nitrite, sulfonates, succinic acids, amines, rust inhibitors typified by carboxylates, and benzotriazoles. Representative metal corrosion inhibitors, fatty agents such as fatty acids, fatty acid esters and phosphate esters, antiwear and extreme pressure agents such as phosphorus, sulfur and organometallics, metal oxides and disulfides Examples thereof include solid lubricants typified by molybdenum. The amount of these components used is usually about 0.1 to 20% by mass, preferably 0.5 to 10% by mass.
〔混和ちょう度〕
 本発明のグリース組成物の混和ちょう度は、使用目的に合わせて調整されるが、好ましくは200~440である。特に軸受用としては、軟らかすぎると漏洩してしまうことが懸念されるため、好ましくは200~350である。
[Mixing consistency]
The penetration of the grease composition of the present invention is adjusted according to the purpose of use, but is preferably 200 to 440. In particular, for bearings, if it is too soft, there is a concern of leakage, so 200 to 350 is preferable.
 本発明のグリース組成物は、各種機械部品に封入して用いることができる。各種機械部品としては、転がり軸受、歯車、ボールネジ、直動軸受、カム又は継ぎ手等が挙げられる。具体的には、産業機械用各種モータ、事務機器用各種モータ、自動車用各種モータ、自動車電装部品や補機部品等に使用される転がり軸受、風車やロボット、自動車などの減速機や増速機等に使用される歯車、電動パワーステアリングや工作機械等に使用されるボールネジ、産業機器や電子機器等に使用される直動軸受、カム又は継ぎ手が挙げられる。 The grease composition of the present invention can be used by being enclosed in various machine parts. Examples of various machine parts include rolling bearings, gears, ball screws, linear motion bearings, cams, and joints. Specifically, various motors for industrial machines, various motors for office equipment, various motors for automobiles, rolling bearings used for automobile electrical parts and auxiliary machine parts, windmills, robots, reduction gears and speed increasers for automobiles, etc. Gears used in the above, ball screws used in electric power steering and machine tools, linear motion bearings used in industrial equipment and electronic equipment, cams or joints.
 <試験グリースの調製>
 表1に示した増ちょう剤及び基油を用い、実施例及び比較例のグリース組成物を調製した。具体的には、基油中で、4,4-ジフェニルメタンジイソシアネートと所定のアミンとを反応させ、昇温、冷却した後、3本ロールミルで混練し、実施例1及び2、及び比較例1~9のグリース組成物を得た。基油としては、JIS K2220 23.に準拠して測定した、40℃における動粘度が70.2mm2/sの合成炭化水素油であるポリ-α-オレフィン油、又は40℃における動粘度が11.6mm2/sのジエステル油であるジオクチルセバケートを用いた。増ちょう剤量は、グリース組成物の混和ちょう度(試験方法JIS K2220 7.)が300になるように調節した。
 上で調製したグリース組成物を、下記の試験方法により評価した。結果を表1に示す。
<Preparation of test grease>
Using the thickener and base oil shown in Table 1, grease compositions of Examples and Comparative Examples were prepared. Specifically, 4,4-diphenylmethane diisocyanate and a predetermined amine are reacted in a base oil, heated and cooled, and then kneaded with a three-roll mill. Examples 1 and 2 and Comparative Examples 1 to 9 grease compositions were obtained. As the base oil, JIS K2220 23. The poly-α-olefin oil is a synthetic hydrocarbon oil having a kinematic viscosity at 40 ° C. of 70.2 mm 2 / s, or a diester oil having a kinematic viscosity at 40 ° C. of 11.6 mm 2 / s. A dioctyl sebacate was used. The amount of the thickener was adjusted so that the grease composition had a blending degree of 300 (test method JIS K2220 7.).
The grease composition prepared above was evaluated by the following test method. The results are shown in Table 1.
<試験方法>
・攪拌抵抗(レオメータ)
 試験は、Anton Paar社製の粘弾性測定装置、Physica MCR301を用いて測定を行った。
 所定のプレートの間に試験グリースを塗布し、所定のプレート間距離に設定した後、はみ出した余分のグリースを除去した。その後、下記に示すせん断速度にて回転させた時のせん断応力を読み取った。
 試験条件を下記に示す。
  せん断速度:1~104-1
  試験温度:25℃
  プレート間距離:0.2mm
  プレート直径:25mm
<評価>
 せん断速度1~104-1におけるせん断応力の平均値を算出し、測定結果とした。
  2000Pa未満・・・合格
  2000Pa以上・・・不合格
<Test method>
・ Agitation resistance (rheometer)
The test was performed using a viscoelasticity measuring device manufactured by Anton Paar, Physica MCR301.
The test grease was applied between the predetermined plates, and after setting the predetermined distance between the plates, the excess grease that protruded was removed. Then, the shear stress when rotating at the shear rate shown below was read.
Test conditions are shown below.
Shear rate: 1 to 10 4 s -1
Test temperature: 25 ° C
Distance between plates: 0.2mm
Plate diameter: 25mm
<Evaluation>
An average value of shear stress at a shear rate of 1 to 10 4 s −1 was calculated and used as a measurement result.
Less than 2000Pa ・ ・ ・ Pass 2000Pa or more ・ ・ ・ Fail
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
 本発明のジウレア増ちょう剤を含有した実施例1及び2のグリース組成物は、せん断応力(=攪拌抵抗)が低く良好であるのに対し、本発明のジウレア増ちょう剤ではない比較例1~9は、せん断応力が高かった。また比較例9は低粘度のジエステル油を基油としているが、本発明のジウレア増ちょう剤ではないため、せん断応力が高かった。 The grease compositions of Examples 1 and 2 containing the diurea thickener of the present invention have good low shear stress (= stirring resistance), while they are not the diurea thickener of the present invention. No. 9 had high shear stress. Comparative Example 9 uses a low-viscosity diester oil as the base oil, but it was not a diurea thickener according to the present invention, and thus the shear stress was high.

Claims (4)

  1.  増ちょう剤と、基油とを含み、前記増ちょう剤が下記式(1)で示されるジウレア化合物であり、かつグリース組成物中の前記増ちょう剤量の割合が3~20質量%であるグリース組成物。
    Figure JPOXMLDOC01-appb-C000001
    (式(1)中、R2は、ジフェニルメタン基を示す。R1及びR3は、同一又は異なっていても良く、シクロへキシル基又は炭素数8~22の直鎖又は分岐アルキル基を示す。式(1)中、シクロへキシル基とアルキル基の総モル数に対するシクロへキシル基のモル数の割合[{(シクロへキシル基の数)/(シクロへキシル基の数+アルキル基の数)}×100]は70~80モル%である。)
    A thickener, a base oil, the thickener is a diurea compound represented by the following formula (1), and the amount of the thickener in the grease composition is 3 to 20% by mass: Grease composition.
    Figure JPOXMLDOC01-appb-C000001
    (In the formula (1), R 2 represents a diphenylmethane group. R 1 and R 3 may be the same or different, and represent a cyclohexyl group or a linear or branched alkyl group having 8 to 22 carbon atoms. In the formula (1), the ratio of the number of moles of cyclohexyl group to the total number of moles of cyclohexyl group and alkyl group [{(number of cyclohexyl groups) / (number of cyclohexyl groups + alkyl group Number)} × 100] is 70 to 80 mol%.)
  2.  増ちょう剤が、式(1)中、アルキル基が炭素数16~20の直鎖アルキル基であるジウレア化合物である、請求項1記載のグリース組成物。 The grease composition according to claim 1, wherein the thickener is a diurea compound in which the alkyl group in the formula (1) is a linear alkyl group having 16 to 20 carbon atoms.
  3.  転がり軸受、歯車、ボールネジ、直動軸受、カム又は継ぎ手に使用される、請求項1又は2記載のグリース組成物。 The grease composition according to claim 1 or 2, which is used for rolling bearings, gears, ball screws, linear motion bearings, cams or joints.
  4.  請求項1~3のいずれか1項記載のグリース組成物を封入した機械部品。 A machine part in which the grease composition according to any one of claims 1 to 3 is enclosed.
PCT/JP2012/054256 2011-02-22 2012-02-22 Grease composition WO2012115141A1 (en)

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JP6348050B2 (en) * 2014-11-05 2018-06-27 日本グリース株式会社 Biodegradable grease composition for wind power generator
CN107207993B (en) 2015-02-05 2020-05-19 出光兴产株式会社 Grease and method for producing grease
WO2017171020A1 (en) * 2016-03-31 2017-10-05 出光興産株式会社 Lubricating oil composition, and precision reduction gear using same
JP6885686B2 (en) 2016-07-26 2021-06-16 協同油脂株式会社 Grease composition
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