JP5028701B2 - Grease composition for constant velocity joint and constant velocity joint - Google Patents
Grease composition for constant velocity joint and constant velocity joint Download PDFInfo
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- JP5028701B2 JP5028701B2 JP2009184663A JP2009184663A JP5028701B2 JP 5028701 B2 JP5028701 B2 JP 5028701B2 JP 2009184663 A JP2009184663 A JP 2009184663A JP 2009184663 A JP2009184663 A JP 2009184663A JP 5028701 B2 JP5028701 B2 JP 5028701B2
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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
- 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
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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
- 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
- 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
- C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
-
- 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
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
-
- 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
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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
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/045—Metal containing thio derivatives
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- 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
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- 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
- C10N2030/76—Reduction of noise, shudder, or vibrations
-
- 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
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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)
Description
本発明は、等速ジョイント(CVJ)用グリース組成物及びこれを封入した等速ジョイントに関する。潤滑される等速ジョイント部分には、極めて高い面圧が発生し、ジョイント部分は、複雑なころがりすべり作用を受ける。このため、異常振動がしばしば発生する。本発明は、このような等速ジョイントを効率よく潤滑し、有効に摩擦を低減して振動の発生を防止し得る等速ジョイント用グリース組成物に関する。 The present invention relates to a grease composition for a constant velocity joint (CVJ) and a constant velocity joint in which the grease composition is enclosed. An extremely high surface pressure is generated in the constant velocity joint portion to be lubricated, and the joint portion is subjected to a complicated rolling and sliding action. For this reason, abnormal vibrations often occur. The present invention relates to a grease composition for a constant velocity joint that can efficiently lubricate such a constant velocity joint and effectively reduce friction to prevent vibrations.
このような等速ジョイントに用いられている潤滑グリースとしては、カルシウムコンプレックス石けんを増ちょう剤とするグリースや、リチウム石けんを増ちょう剤とし、例えば、硫化油脂、トリクレジルホスフェート、及びジチオリン酸亜鉛からなる群から選択された硫黄−リン系極圧剤を含有したグリースが挙げられる。
最近の自動車工業においては、車両の環境対策(CO2削減)を目的とした軽量化かつ居住空間の確保の点から、4輪駆動(FFタイプ)車が急激に増加し、これに不可欠な等速ジョイント(CVJ)が広く用いられている。このCVJの中で、プランジング型等速ジョイント、特にトリポート型等速ジョイント(TJ)、ダブルオフセット型等速ジョイント(DOJ)等は、ある角度の付いた状態で、回転時に複雑なころがりすべり運動を行うため、軸方向にスライド抵抗を生じ、これがアイドリング時の振動、発進及び加速時の車体の横揺れ、特定速度での車内でのビート音、又はこもり音の起振源となっている。この問題の解決のため、種々の等速ジョイント(CVJ)自体の構造の改良もなされているが、ジョイントの占めるスペース、重さ、及びコスト面でその改良は難しく、振動低減性能に優れたグリースが要求されている。
Lubricating greases used in such constant velocity joints include greases using calcium complex soap as a thickener and lithium soaps as a thickener, such as sulfurized fats and oils, tricresyl phosphate, and zinc dithiophosphate. Grease containing a sulfur-phosphorus extreme pressure agent selected from the group consisting of:
In the recent automobile industry, the number of four-wheel drive (FF type) vehicles has increased rapidly in order to reduce the weight and secure living space for the purpose of environmental measures (CO 2 reduction) for vehicles. Fast joints (CVJ) are widely used. Among these CVJs, plunging type constant velocity joints, especially tripod type constant velocity joints (TJ), double offset type constant velocity joints (DOJ), etc., have a complicated rolling sliding motion at an angle. For this reason, a slide resistance is generated in the axial direction, and this becomes a vibration source for idling vibration, vehicle body roll at start and acceleration, beat sound in a vehicle at a specific speed, or a booming sound. In order to solve this problem, various constant velocity joints (CVJs) themselves have been improved in structure, but it is difficult to improve the space, weight, and cost of the joints, and the grease has excellent vibration reduction performance. Is required.
このため、ウレア系増ちょう剤、二硫化モリブデン、及び 酸化ワックスのカルシウム塩、石油スルホン酸のカルシウム塩、アルキル芳香族スルホン酸のカルシウム塩、サリシレートのカルシウム塩、フェネートのカルシウム塩、酸化ワックスの過塩基性カルシウム塩、石油スルホン酸の過塩基性カルシウム塩、アルキル芳香族スルホン酸の過塩基性カルシウム塩、サリシレートの過塩基性カルシウム塩、及びフェネートの過塩基性カルシウム塩からなる群から選択される少なくとも1種を含有する等速ジョイント用グリース組成物(特許文献1)や、さらにこれらの成分に加え、金属を含まない硫黄−リン系極圧剤、及びモリブデンジチオカーバメートを含有する等速ジョイント用グリース組成物(特許文献2)が提案されている。
また、基油、ジウレア系増ちょう剤、二硫化モリブデン、硫化ジアルキルジチオカルバミン酸モリブデン、石油スルホン酸のカルシウム塩、硫黄−リン系極圧剤、及び植物性油脂を含有する等速ジョイント用組成物も提案されている(特許文献3)。
しかし、従来の等速ジョイント用グリース組成物は、その摩擦係数低減効果及び振動発生防止効果は必ずしも十分とはいえない。
For this reason, urea-based thickeners, molybdenum disulfide, and calcium oxide oxide wax, calcium salt of petroleum sulfonic acid, calcium salt of alkyl aromatic sulfonic acid, calcium salt of salicylate, calcium salt of phenate, excess of oxidized wax. Selected from the group consisting of basic calcium salt, petroleum sulfonic acid overbased calcium salt, alkyl aromatic sulfonic acid overbased calcium salt, salicylate overbased calcium salt, and phenate overbased calcium salt Grease composition for constant velocity joints containing at least one (Patent Document 1), and further for these constant velocity joints containing a metal-free sulfur-phosphorus extreme pressure agent and molybdenum dithiocarbamate in addition to these components A grease composition (Patent Document 2) has been proposed.
There is also a constant velocity joint composition containing a base oil, a diurea thickener, molybdenum disulfide, molybdenum disulfide dialkyldithiocarbamate, a calcium salt of petroleum sulfonic acid, a sulfur-phosphorus extreme pressure agent, and vegetable oils and fats. It has been proposed (Patent Document 3).
However, the conventional grease composition for constant velocity joints is not necessarily sufficient in the friction coefficient reduction effect and the vibration generation prevention effect.
従って、本発明の目的は、等速ジョイント用グリース組成物、特に、等速ジョイントを効率よく潤滑し、有効に摩擦を低減し振動の発生を防止し得る等速ジョイント用グリース組成物、及びこれを封入した等速ジョイントを提供することである。 Accordingly, an object of the present invention is to provide a grease composition for a constant velocity joint, in particular, a grease composition for a constant velocity joint that can efficiently lubricate the constant velocity joint, effectively reduce friction and prevent vibrations, and the like. It is to provide a constant velocity joint encapsulating.
本発明者等は、等速ジョイントの摩擦を低減し、振動を防止するグリース組成物の開発研究を種々行い、振動の発生し易い潤滑条件下で便用するグリースの性能評価を、振動摩擦摩耗試験機として知られるSRV試験機を用いて行った。その結果、等速ジョイントを起振源とした振動と、SRV試験機で測定した特定の振動条件下の摩擦係数に特別な関係があることを見いだした。さらに、本発明者等は、基グリースにウレアグリースを用いて、油性剤及び各種極圧剤等の様々な組み合わせによって、上述の関係を検討した。その結果、基油、ウレア系増ちょう剤、パームオレイン、パームステアリン及びグリセリンモノオレエートからなる群から選ばれる少なくとも1種の油性剤、硫化ジアルキルジチオカルバミン酸モリブデン、亜鉛スルホネートおよび硫黄−リン系極圧剤を含有するグリース組成物が、低摩擦係数の望ましい潤滑特性を示すことを見いだし、さらに、実際の等速ジョイントを用いた強制力試験においても、従来の等速ジョイント用グリースとは異なり、振動の発生を顕著に防止し得ることを確認し、本発明を完成するに至った。 The present inventors have conducted various researches on the development of grease compositions that reduce the friction of constant velocity joints and prevent vibrations, and evaluated the performance of greases used for stool under lubrication conditions where vibrations are likely to occur. An SRV tester known as a tester was used. As a result, we found that there is a special relationship between the vibration with constant velocity joint as the vibration source and the friction coefficient measured by SRV test machine under specific vibration conditions. Furthermore, the present inventors examined the above relationship by using urea grease as the base grease and various combinations of oil-based agents and various extreme pressure agents. As a result, at least one oily agent selected from the group consisting of base oils, urea thickeners, palm olein, palm stearin and glycerin monooleate, molybdenum dialkyldithiocarbamate sulfide, zinc sulfonate and sulfur-phosphorus extreme pressure It was found that the grease composition containing the agent exhibits desirable lubrication characteristics with a low coefficient of friction, and even in a forced force test using an actual constant velocity joint, unlike conventional constant velocity joint grease, vibration As a result, it was confirmed that the occurrence of water vapor can be remarkably prevented, and the present invention has been completed.
本発明は、上記知見に基づいてなされたもので、下記の等速ジョイント用グリース組成物及びこれを封入した等速ジョイントを提供するものである。
1.下記の成分を含有する等速ジョイント用グリース組成物。
(a)基油、
(b)ジウレア系増ちょう剤、
(c)パームオレイン、パームステアリン及びグリセリンモノオレエートからなる群から選ばれる少なくとも1種の油性剤、
(d)次式で表される硫化ジアルキルジチオカルバミン酸モリブデン、
(R3R4N−CS−S)2−Mo2OmSn
(式中、R3及びR4は独立して、炭素数1〜24のアルキル基を表し、mは0〜3、nは4〜1であり、m+n=4である。)
(e)亜鉛スルホネート、及び
(f)硫黄−リン系極圧添加剤。
2.ジウレア系増ちょう剤が次式で表されるジウレア系増ちょう剤であることを特徴とする上記1記載の等速ジョイント用グリース組成物。
R1-NH-CO-NH-C6H4-p-CH2-C6H4-p-NH-CO-NHR2
(R1及びR2は独立して、炭素原子数8〜18のアルキル基である。)
3.パームオレインの沃素価が56〜72及び上昇融点が24℃以下であることを特徴とする上記1記載の等速ジョイント用グリース組成物。
4.パームステアリンの沃素価が48以下及び上昇融点が44℃以上であることを特徴とする上記1記載の等速ジョイント用グリース組成物。
5.全組成物中における各成分の含有量が、
(a)基油49.0〜98.65質量%、
(b)ジウレア系増ちょう剤1.0〜25.0質量%、
(c)油性剤0.1〜5.0質量%、
(d)硫化ジアルキルジチオカルバミン酸モリブデン0.1〜5.0質量%、
(e)亜鉛スルホネート0.1〜15.0質量%、及び
(f)硫黄−リン系極圧添加剤0.05〜1.0質量%
である上記1又は2記載の等速ジョイント用グリース組成物。
6.プランジング型等速ジョイント用である上記1〜5のいずれか1項記載の等速ジョイント用グリース組成物。
7.上記1〜6のいずれか1項記載の等速ジョイント用グリース組成物を封入した等速ジョイント。
The present invention has been made based on the above findings, and provides the following grease composition for a constant velocity joint and a constant velocity joint in which the grease composition is enclosed.
1. A grease composition for a constant velocity joint containing the following components:
(A) base oil,
(B) a diurea thickener;
(C) at least one oily agent selected from the group consisting of palm olein, palm stearin and glycerin monooleate;
(D) molybdenum disulfide dialkyldithiocarbamate represented by the following formula:
(R 3 R 4 N-CS -S) 2 -Mo 2 O m S n
(In the formula, R 3 and R 4 independently represent an alkyl group having 1 to 24 carbon atoms, m is 0 to 3, n is 4 to 1, and m + n = 4.)
(E) Zinc sulfonate, and (f) Sulfur-phosphorus extreme pressure additive.
2. 2. The grease composition for a constant velocity joint as described in 1 above, wherein the diurea thickener is a diurea thickener represented by the following formula.
R 1 -NH-CO-NH-C 6 H 4 -p-CH 2 -C 6 H 4 -p-NH-CO-NHR 2
(R 1 and R 2 are independently an alkyl group having 8 to 18 carbon atoms.)
3. 2. The grease composition for a constant velocity joint as described in 1 above, wherein the iodine value of palm olein is 56 to 72 and the rising melting point is 24 ° C. or lower.
4). 2. The grease composition for constant velocity joints according to 1 above, wherein the iodine value of palm stearin is 48 or less and the rising melting point is 44 ° C. or more.
5. The content of each component in the entire composition is
(A) 49.0 to 98.65% by mass of base oil,
(B) 1.0 to 25.0% by mass of a diurea thickener;
(C) Oiliness agent 0.1-5.0 mass%,
(D) 0.1 to 5.0% by mass of molybdenum dialkyldithiocarbamate sulfide,
(E) Zinc sulfonate 0.1 to 15.0% by mass, and (f) Sulfur-phosphorus extreme pressure additive 0.05 to 1.0% by mass.
The grease composition for constant velocity joints according to 1 or 2 above.
6). 6. The grease composition for a constant velocity joint according to any one of 1 to 5 above, which is for a plunging type constant velocity joint.
7). The constant velocity joint which enclosed the grease composition for constant velocity joints of any one of said 1-6.
本発明の等速ジョイント用グリース組成物は、等速ジョイントを効率よく潤滑し、有効に摩擦を低減し、振動の発生を顕著に防止し得る。また従来の等速ジョイント用グリース組成物と比較して耐ジョイントフレーキング特性に優れている。 The grease composition for a constant velocity joint of the present invention can efficiently lubricate the constant velocity joint, effectively reduce friction, and remarkably prevent the occurrence of vibration. In addition, it has superior joint flaking resistance compared to conventional grease compositions for constant velocity joints.
以下、本発明の等速ジョイント用グリース組成物について詳述する。
本発明のグリース組成物は、下記成分(a)、(b)、(c)、(d)、(e)、及び(f)を含有する。
(a)基油、
(b)ジウレア系増ちょう剤、
(c)パームオレイン、パームステアリン及びグリセリンモノオレエートからなる群から選ばれる少なくとも1種の油性剤、
(d)次式で表される硫化ジアルキルジチオカルバミン酸モリブデン、
(R3R4N−CS−S)2−Mo2OmSn
(式中、R3及びR4は独立して、炭素数1〜24のアルキル基を表し、mは0〜3、nは4〜1であり、m+n=4である。)
(e)亜鉛スルホネート、及び
(f)硫黄−リン系極圧剤
Hereinafter, the grease composition for constant velocity joints of the present invention will be described in detail.
The grease composition of the present invention contains the following components (a), (b), (c), (d), (e), and (f).
(A) base oil,
(B) a diurea thickener;
(C) at least one oily agent selected from the group consisting of palm olein, palm stearin and glycerin monooleate;
(D) molybdenum disulfide dialkyldithiocarbamate represented by the following formula:
(R 3 R 4 N-CS -S) 2 -Mo 2 O m S n
(In the formula, R 3 and R 4 independently represent an alkyl group having 1 to 24 carbon atoms, m is 0 to 3, n is 4 to 1, and m + n = 4.)
(E) zinc sulfonate and (f) sulfur-phosphorus extreme pressure agent
上記(a)成分の基油としては、鉱物油、エーテル系合成油、エステル系合成油及び炭化水素系合成油等の通常に使用されている潤滑油またはそれらの混合油が挙げられるが、これらに限定されるものではない。コストの点から、鉱物油を用いるのが好ましく、また、鉱物油を主成分とし、これに合成油を混合した基油を用いるのが好ましい。
上記基油の100℃における動粘度は、好ましくは5〜30mm2/sであり、より好ましくは7〜20mm2/sである。5mm2/s未満では、等速ジョイント(CVJ)内で油膜を形成せず高速耐久性が不充分となる傾向があり、30mm2/sを超えるとCVJ内の発熱のため高速耐久性が低下する傾向がある。
Examples of the base oil of the component (a) include commonly used lubricating oils such as mineral oils, ether-based synthetic oils, ester-based synthetic oils and hydrocarbon-based synthetic oils, or mixed oils thereof. It is not limited to. From the viewpoint of cost, it is preferable to use a mineral oil, and it is preferable to use a base oil in which a mineral oil is a main component and a synthetic oil is mixed.
The kinematic viscosity at 100 ° C. of the base oil is preferably 5 to 30 mm 2 / s, more preferably 7 to 20 mm 2 / s. If it is less than 5 mm 2 / s, oil film is not formed in the constant velocity joint (CVJ) and high-speed durability tends to be insufficient, and if it exceeds 30 mm 2 / s, high-speed durability decreases due to heat generation in the CVJ. Tend to.
上記(b)成分のジウレア系増ちょう剤は全て使用することができる。好ましくは、下記の式で表されるものが挙げられる。
R1-NH-CO-NH-C6H4-p-CH2-C6H4-p-NH-CO-NHR2
(R1及びR2は独立して、炭素原子数8〜18のアルキル基である。)
上記ジウレア系増ちょう剤は、ジフェニルメタンジイソシアネートと炭素数8〜18のアルキルアミン、例えば、オクチルアミン、ドデシルアミン、ヘキサデシルアミン、オクタデシルアミン等との反応により得られる。上記ジイソシアネートとアミンとを反応させる方法には特に制限はなく、従来公知の方法により実施することができる。
Any of the diurea thickeners of component (b) can be used. Preferably, what is represented by a following formula is mentioned.
R 1 -NH-CO-NH-C 6 H 4 -p-CH 2 -C 6 H 4 -p-NH-CO-NHR 2
(R 1 and R 2 are independently an alkyl group having 8 to 18 carbon atoms.)
The diurea thickener is obtained by reacting diphenylmethane diisocyanate with an alkylamine having 8 to 18 carbon atoms such as octylamine, dodecylamine, hexadecylamine, octadecylamine and the like. There is no restriction | limiting in particular in the method of making the said diisocyanate and amine react, It can implement by a conventionally well-known method.
上記(c)成分の油性剤は、パームオレイン、パームステアリン及びグリセリンモノオレエートからなる群から選ばれる少なくとも1種である。特にパームオレイン、パームステアリンが好ましい。パームオレイン(palm olein)及びパームステアリン(palm stearin)は、一般的にアブラヤシの果肉(油脂含量16〜20%)から圧搾によって得られる油脂を分別し、必要な性状をもつ油脂分に分けたパーム分別油であり、潤滑作用に有効である。
パーム分別油には、低融点画分のパームオレインと高融点画分のパームステアリンがある。JAS規格では、パームオレインは酸価0.20以下、水分夾雑物0.1%以下、ヨウ素価56〜72、上昇融点24℃以下等となっており、パームステアリンは酸価0.20以下、水分夾雑物0.10%以下、ヨウ素価48以下、上昇融点44℃以上等となっている。また、パームオレインは40℃で清澄なもの、パームステアリンは60℃で清澄なものとなっている。
本発明のグリース組成物に使用するパームオレインは、好ましくは、ヨウ素価が56〜72及び上昇融点が24℃以下のものであり、さらに好ましくはヨウ素価が60〜72及び上昇融点が20℃以下、最も好ましくはヨウ素価が65〜70及び上昇融点が13℃以下のものである。
本発明のグリース組成物に使用するパームステアリンは、好ましくはヨウ素価が48以下及び上昇融点が44℃以上のものであり、さらに好ましくはヨウ素価が22〜48及び上昇融点が44〜56℃のものである。
The oily agent as the component (c) is at least one selected from the group consisting of palm olein, palm stearin and glycerin monooleate. Palm olein and palm stearin are particularly preferable. Palm olein (palm olein) and palm stearin (palm stearin) are generally obtained by separating oils and fats obtained by pressing from oil palm pulp (oils and fats content of 16 to 20%) and dividing them into oils and fats having the necessary properties. It is a fractionated oil and is effective for lubrication.
Palm fractionated oils include palm olein in the low melting fraction and palm stearin in the high melting fraction. In the JAS standard, palm olein has an acid value of 0.20 or less, moisture impurities of 0.1% or less, iodine value of 56 to 72, rising melting point of 24 ° C. or less, and palm stearin has an acid value of 0.20 or less, The moisture content is 0.10% or less, the iodine value is 48 or less, the rising melting point is 44 ° C. or more, and the like. Palm olein is clear at 40 ° C., and palm stearin is clear at 60 ° C.
The palm olein used in the grease composition of the present invention preferably has an iodine value of 56 to 72 and an increasing melting point of 24 ° C. or less, more preferably an iodine value of 60 to 72 and an increasing melting point of 20 ° C. or less. Most preferably, the iodine value is 65 to 70 and the rising melting point is 13 ° C. or less.
The palm stearin used in the grease composition of the present invention preferably has an iodine value of 48 or less and an ascending melting point of 44 ° C or more, more preferably an iodine value of 22 to 48 and an ascending melting point of 44 to 56 ° C. Is.
上記(d)成分は、次式で表される硫化ジアルキルジチオカルバミン酸モリブデンである。
(R3R4N−CS−S)2−Mo2OmSn
(式中、R3及びR4は独立して、炭素数1〜24のアルキル基を表し、mは0〜3、nは4〜1であり、m+n=4である。)
R3及びR4は、独立して、炭素数1〜24、好ましくは炭素数2〜18のアルキル基である。
上記(e)成分の亜鉛スルホネートの塩基価は、好ましくは50mgKOH/g以下、さらに好ましくは40mgKOH/g以下であり、例えば、塩基価50mgKOH/g以下のジノニルナフタレンスルホン酸の亜鉛塩が挙げられる。これらの亜鉛塩は、エンジン油等の潤滑油に用いられる金属系清浄分散剤や防錆剤として知られている、潤滑油留分中の芳香族炭化水素成分のスルホン化によって得られる。
The component (d) is a molybdenum dialkyldithiocarbamate sulfide represented by the following formula.
(R 3 R 4 N-CS -S) 2 -Mo 2 O m S n
(In the formula, R 3 and R 4 independently represent an alkyl group having 1 to 24 carbon atoms, m is 0 to 3, n is 4 to 1, and m + n = 4.)
R 3 and R 4 are each independently an alkyl group having 1 to 24 carbon atoms, preferably 2 to 18 carbon atoms.
The base number of the zinc sulfonate as the component (e) is preferably 50 mgKOH / g or less, more preferably 40 mgKOH / g or less, for example, a zinc salt of dinonylnaphthalenesulfonic acid having a base number of 50 mgKOH / g or less. . These zinc salts are obtained by sulfonation of aromatic hydrocarbon components in the lubricating oil fraction, which are known as metallic detergents and rust inhibitors used in lubricating oils such as engine oils.
上記(f)成分の、硫黄−リン系極圧剤として好ましいものは、硫黄分15〜35重量%及びリン分0.5〜3質量%のものであり、硫黄成分とリン成分の比率を調整することにより、優れた摩耗防止性能や焼き付き防止性能を発揮させることができる。硫黄成分が上記範囲より多いとジョイントが腐食し易くなり、リン成分が上記範囲より多いとジョイントの摩耗防止効果が得られ難くなる。また両者とも上記範囲より少ない場合は、目的とする摩耗防止性能や焼き付き防止性能を十分に発揮させることが困難になる。 The component (f) is preferably a sulfur-phosphorus extreme pressure agent having a sulfur content of 15 to 35% by weight and a phosphorus content of 0.5 to 3% by mass, and adjusting the ratio of the sulfur component and the phosphorus component. By doing so, excellent wear prevention performance and anti-seizure performance can be exhibited. If the sulfur component is more than the above range, the joint is easily corroded, and if the phosphorus component is more than the above range, it is difficult to obtain the joint wear prevention effect. Moreover, when both are less than the said range, it will become difficult to fully exhibit the target wear prevention performance and image sticking prevention performance.
本発明の等速ジョイント用グリース組成物において、等速ジョイント用グリース組成物の全質量に対して、(a)成分の基油の含有量は、好ましくは49.0〜98.65質量%、(b)成分のジウレア系増ちょう剤の含有量は、好ましくは1.0〜25.0質量%、さらに好ましくは5.0〜15.0質量%、(c)パームオレイン、パームステアリン及びグリセリンモノオレエートからなる群から選ばれる少なくとも1種の油性剤の含有量は、好ましくは0.1〜5.0質量%、さらに好ましくは0.5〜5.0質量%、(d)成分の硫化ジアルキルジチオカルバミン酸モリブデンの含有量は、好ましくは0.1〜5.0質量%、さらに好ましくは0.5〜5.0質量%、(e)成分のスルホン酸亜鉛の含有量は、好ましくは0.1〜15.0質量%、さらに好ましくは1.0〜13.0質量%、(f)成分の硫黄−リン系極圧剤の含有量は、好ましくは0.05〜1.0質量%、さらに好ましくは0.1〜1.0質量%である。 In the grease composition for constant velocity joints of the present invention, the content of the base oil of component (a) is preferably 49.0 to 98.65% by mass with respect to the total mass of the grease composition for constant velocity joints, The content of the diurea thickener as component (b) is preferably 1.0 to 25.0 mass%, more preferably 5.0 to 15.0 mass%, (c) palm olein, palm stearin and glycerin. The content of at least one oily agent selected from the group consisting of monooleate is preferably 0.1 to 5.0% by mass, more preferably 0.5 to 5.0% by mass, The content of molybdenum sulfide dialkyldithiocarbamate is preferably 0.1 to 5.0% by mass, more preferably 0.5 to 5.0% by mass, and the content of zinc sulfonate as component (e) is preferably 0.1-1 0.0 mass%, more preferably 1.0-13.0 mass%, the content of the sulfur-phosphorus extreme pressure agent of component (f) is preferably 0.05-1.0 mass%, more preferably 0.1 to 1.0% by mass.
上記(b)成分のジウレア系増ちょう剤の含有量が1.0質量%未満であると、増ちょう効果が少なく、グリース化しにくくなり、25.0質量%を越えると、得られた組成物が硬くなりすぎ、所期の効果が得られなくなる場合があるので、上記範囲内とすることが好ましい。
上記(c)成分の油性剤の含有量が0.1質量%未満であると、所期の効果を得ることが困難になり、5.0質量%を越えて含有させても効果の増大がない場合があるので、上記範囲内とすることが好ましい。
上記(d)成分の硫化ジアルキルジチオカルバミン酸モリブデンの含有量が0.1質量%未満であると、所期の効果を得ることが困難になり、5.0質量%を越えて含有させても効果の増大がない場合があるので、上記範囲内とすることが好ましい。
上記(e)成分のスルホン酸亜鉛の含有量が0.1質量%未満であると、所期の効果を得ることが困難になり、15.0質量%を越えて含有させても効果の増大がない場合があるので、上記範囲内とすることが好ましい。
上記(f)成分の硫黄−リン系極圧剤の含有量が0.05質量%未満であると、所期の効果を得ることが困難になり、1.0質量%を越えて含有させても効果の増大がない場合があるので、上記範囲内とすることが好ましい。
When the content of the diurea thickener as the component (b) is less than 1.0% by mass, the thickening effect is small and it becomes difficult to form a grease. When the content exceeds 25.0% by mass, the resulting composition is obtained. Is too hard, and the desired effect may not be obtained.
When the content of the oily agent as the component (c) is less than 0.1% by mass, it is difficult to obtain the desired effect, and even if the content exceeds 5.0% by mass, the effect is increased. Since it may not be, it is preferable to be within the above range.
When the content of molybdenum sulfide dialkyldithiocarbamate as the component (d) is less than 0.1% by mass, it becomes difficult to obtain the desired effect, and even if the content exceeds 5.0% by mass, the effect is achieved. Since there is a case where there is no increase in the thickness, it is preferable to be within the above range.
When the content of zinc sulfonate as the component (e) is less than 0.1% by mass, it is difficult to obtain the desired effect, and even if the content exceeds 15.0% by mass, the effect is increased. Therefore, it is preferable to be within the above range.
When the content of the sulfur-phosphorus extreme pressure agent as the component (f) is less than 0.05% by mass, it becomes difficult to obtain the desired effect, and the content exceeds 1.0% by mass. Since there is a case where the effect does not increase, it is preferable to be within the above range.
本発明の等速ジョイント用グリース組成物には、上記(a)〜(f)成分に加え、更に各種潤滑油やグリースに一般的に用いられている酸化防止剤、防錆剤、ポリマー添加剤を添加することができる。また、上記成分以外の極圧剤、摩擦緩和剤、耐摩耗剤及び固体潤滑剤等の添加剤を添加することができる。上記添加剤を添加する場合、その含有量は、等速ジョイント用グリース組成物の全質量中、好ましくは0.1〜10.0質量%である。 In addition to the above components (a) to (f), the grease composition for constant velocity joints of the present invention further includes antioxidants, rust inhibitors and polymer additives generally used in various lubricating oils and greases. Can be added. In addition to the above components, additives such as extreme pressure agents, friction modifiers, antiwear agents and solid lubricants can be added. When the above additive is added, the content thereof is preferably 0.1 to 10.0% by mass in the total mass of the grease composition for constant velocity joints.
以下、本発明を実施例により更に詳細に説明する。なお、本発明の範囲は、かかる実施例に限定されないことはいうまでもない。
実施例1
容器に基油440gとジフェニルメタン−4,4′−ジイソシアネート58.9gをとり、混合物を70〜80℃に加熱した。別容器に基油440gとオクチルアミン61.1gをとり、70〜80℃に加熱後、先の容器に加え、よく攪拌しながら、30分間反応させた。その後攪拌しながら、160℃まで昇温し、放冷後、ベース脂肪族アミンジウレアグリースを得た。このベースグリースに、表1に示す配合で、添加剤を添加し、適宜基油を加え、得られる混合物を三段ロールミルにて、ちょう度No. 1 グレードに調整した。
グリースの基油として、以下の特性を有する鉱油を使用した。
粘度 40℃ 157 mm2/s
100℃ 14 mm2/s
粘度指数 88
Hereinafter, the present invention will be described in more detail with reference to examples. Needless to say, the scope of the present invention is not limited to such examples.
Example 1
A container was charged with 440 g of base oil and 58.9 g of diphenylmethane-4,4′-diisocyanate, and the mixture was heated to 70-80 ° C. In a separate container, 440 g of base oil and 61.1 g of octylamine were taken, heated to 70-80 ° C., added to the previous container, and allowed to react for 30 minutes with good stirring. Thereafter, the temperature was raised to 160 ° C. while stirring, and after cooling, a base aliphatic amine diurea grease was obtained. Additives were added to this base grease in the formulation shown in Table 1, base oil was added as appropriate, and the resulting mixture was adjusted to a consistency No. 1 grade with a three-stage roll mill.
A mineral oil having the following characteristics was used as the base oil of the grease.
Viscosity 40 ° C 157 mm 2 / s
100 ° C 14 mm 2 / s
Viscosity index 88
表1及び表2に実施例1〜13及び表3〜表5に比較例1〜24を示す。
実施例1〜13において、各々の成分(c)、成分(d)、成分(e)、成分(f)を添加しなかった他は同様にした比較例1〜23のグリースを調製した。
比較例24は市販のMoDTCを含有するウレアグリースである。
なお、表中に示す各成分は以下のとおりであり、表中の数字は質量%を示す。
MoDTC(硫化ジアルキルジチオカルバミン酸モリブデン):商品名サクラルーブ600(旭電化工業社製)
パームオレイン :パームオレイン100%、沃素価66〜70、上昇融点13℃以下
パームステアリン:パームステアリン100%、沃素価22〜48、上昇融点44〜56℃
亜鉛スルホネート :ジノニルナフタレンスルホン酸亜鉛(塩基価50mgKOH/g以下)
硫黄−リン系極圧添加剤 :商品名:ルブリゾール810(日本ルブリゾール社製)
Tables 1 and 2 show Examples 1 to 13 and Tables 3 to 5 show Comparative Examples 1 to 24.
The greases of Comparative Examples 1 to 23 were prepared in the same manner as in Examples 1 to 13, except that each component (c), component (d), component (e), and component (f) were not added.
Comparative Example 24 is a commercially available urea grease containing MoDTC.
In addition, each component shown in the table | surface is as follows, and the number in a table | surface shows the mass%.
MoDTC (molybdenum dialkyldithiocarbamate): Brand name SakuraLube 600 (Asahi Denka Kogyo Co., Ltd.)
Palm olein: 100% palm olein, iodine value 66-70, rising melting point 13 ° C. or less Palm stearin: 100% palm stearin, iodine value 22-48, rising melting point 44-56 ° C.
Zinc sulfonate: zinc dinonylnaphthalene sulfonate (base number 50 mgKOH / g or less)
Sulfur-phosphorus extreme pressure additive: Trade name: Lubrizol 810 (manufactured by Nippon Lubrizol)
上記等速ジョイント用グリース組成物につき、以下に示す試験方法で物性の評価を行った。
SRV試験
テストピース ボール :直径17.5mm(SUJ2)
プレート:直径24mm×7.85mm(SUJ2)
試験条件 荷重 :200N
周波数 :50Hz
振幅 :0.8mm
時間 :10分
試験温度:40℃
測定項目 摩擦係数(μ)
強制力試験
下記条件にて実ジョイントでの強制力試験を行い、強制力を測定した。
試験条件 回転数:200rpm
トルク:500Nm
ジョイント角度:10°
運転時間:2min.
ジョイントタイプ:トリポート型等速ジョイント
測定項目 ジョイント強制力を測定し、市販ウレアグリースを基準としての増減率(%)で評価した。
The physical properties of the grease composition for constant velocity joints were evaluated by the following test methods.
SRV test test piece Ball: 17.5mm in diameter (SUJ2)
Plate: Diameter 24mm x 7.85mm (SUJ2)
Test conditions Load: 200N
Frequency: 50Hz
Amplitude: 0.8 mm
Time: 10 minutes
Test temperature: 40 ° C
Measurement item Friction coefficient (μ)
Force test
The forcible force test at the actual joint was performed under the following conditions, and the forcible force was measured.
Test conditions Rotation speed: 200rpm
Torque: 500Nm
Joint angle: 10 °
Operating time: 2 min.
Joint type: Tripport type constant velocity joint Measurement item The joint forcing force was measured and evaluated by the rate of change (%) based on commercially available urea grease.
成分(c)〜(f)を含有する本発明の実施例1〜13のグリース組成物は、成分(c)〜(f)のいずれかの成分を含まない比較例1〜20のグリース組成物および比較例21の市販品と比較して、著しい摩擦係数低減効果及び振動発生防止効果を示すことがわかる。 The grease compositions of Examples 1 to 13 of the present invention containing the components (c) to (f) are the grease compositions of Comparative Examples 1 to 20 that do not contain any of the components (c) to (f). It can be seen that, compared with the commercial product of Comparative Example 21, a remarkable friction coefficient reduction effect and vibration generation prevention effect are exhibited.
Claims (7)
(a)基油、
(b)ジウレア系増ちょう剤、
(c)パームオレイン、パームステアリン及びグリセリンモノオレエートからなる群から選ばれる少なくとも1種の油性剤、
(d)次式で表される硫化ジアルキルジチオカルバミン酸モリブデン、
(R3R4N−CS−S)2−Mo2OmSn
(式中、R3及びR4は独立して、炭素数1〜24のアルキル基を表し、mは0〜3、nは4〜1であり、m+n=4である。)
(e)亜鉛スルホネート、及び
(f)硫黄−リン系極圧添加剤。 A grease composition for a constant velocity joint containing the following components:
(A) base oil,
(B) a diurea thickener;
(C) at least one oily agent selected from the group consisting of palm olein, palm stearin and glycerin monooleate;
(D) molybdenum disulfide dialkyldithiocarbamate represented by the following formula:
(R 3 R 4 N-CS -S) 2 -Mo 2 O m S n
(In the formula, R 3 and R 4 independently represent an alkyl group having 1 to 24 carbon atoms, m is 0 to 3, n is 4 to 1, and m + n = 4.)
(E) Zinc sulfonate, and (f) Sulfur-phosphorus extreme pressure additive.
R1-NH-CO-NH-C6H4-p-CH2-C6H4-p-NH-CO-NHR2
(R1及びR2は独立して、炭素原子数8〜18のアルキル基である。) The grease composition for a constant velocity joint according to claim 1, wherein the diurea thickener is a diurea thickener represented by the following formula.
R 1 -NH-CO-NH-C 6 H 4 -p-CH 2 -C 6 H 4 -p-NH-CO-NHR 2
(R 1 and R 2 are independently an alkyl group having 8 to 18 carbon atoms.)
(a)基油49.0〜98.65質量%、
(b)ジウレア系増ちょう剤1.0〜25.0質量%、
(c)油性剤0.1〜5.0質量%、
(d)硫化ジアルキルジチオカルバミン酸モリブデン0.1〜5.0質量%、
(e)亜鉛スルホネート0.1〜15.0質量%、及び
(f)硫黄−リン系極圧添加剤0.05〜1.0質量%
である請求項1又は2記載の等速ジョイント用グリース組成物。 The content of each component in the entire composition is
(A) 49.0 to 98.65% by mass of base oil,
(B) 1.0 to 25.0% by mass of a diurea thickener,
(C) Oiliness agent 0.1-5.0 mass%,
(D) 0.1 to 5.0% by mass of molybdenum dialkyldithiocarbamate sulfide,
(E) Zinc sulfonate 0.1 to 15.0% by mass, and (f) Sulfur-phosphorus extreme pressure additive 0.05 to 1.0% by mass.
The grease composition for constant velocity joints according to claim 1 or 2.
Priority Applications (4)
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JP2009184663A JP5028701B2 (en) | 2009-08-07 | 2009-08-07 | Grease composition for constant velocity joint and constant velocity joint |
KR1020127000947A KR20120028976A (en) | 2009-08-07 | 2010-08-09 | Grease composition for constant velocity joints, and constant velocity joint |
PCT/JP2010/063453 WO2011016580A1 (en) | 2009-08-07 | 2010-08-09 | Grease composition for constant velocity joints, and constant velocity joint |
CN2010800347835A CN102471722A (en) | 2009-08-07 | 2010-08-09 | Grease composition for constant velocity joints, and constant velocity joint |
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JP2009184663A JP5028701B2 (en) | 2009-08-07 | 2009-08-07 | Grease composition for constant velocity joint and constant velocity joint |
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JP2011037950A JP2011037950A (en) | 2011-02-24 |
JP5028701B2 true JP5028701B2 (en) | 2012-09-19 |
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JP (1) | JP5028701B2 (en) |
KR (1) | KR20120028976A (en) |
CN (1) | CN102471722A (en) |
WO (1) | WO2011016580A1 (en) |
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KR102099167B1 (en) * | 2012-10-05 | 2020-04-09 | 교도유시 가부시끼가이샤 | Grease composition |
JP6601606B2 (en) * | 2014-12-18 | 2019-11-06 | 協同油脂株式会社 | Grease composition |
KR101980635B1 (en) * | 2015-03-31 | 2019-05-22 | 게케엔 드리펠린 인터나쇼날 게엠베하 | Grease composition for use in constant velocity joints |
EP4253507A4 (en) | 2020-11-26 | 2024-04-17 | Kyodo Yushi | Grease composition for constant-velocity joint |
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TW200624549A (en) * | 2004-11-08 | 2006-07-16 | Thk Co Ltd | Grease composition conforming to vibration and guide employing the same |
JP4809603B2 (en) * | 2004-11-25 | 2011-11-09 | 本田技研工業株式会社 | Constant velocity joint |
US20080295391A1 (en) * | 2005-07-25 | 2008-12-04 | C.M. Intellectual Property And Research, Inc. | Fuel and Lubricant Additives and Methods for Improving Fuel Economy and Vehicle Emissions |
JP2008297447A (en) * | 2007-05-31 | 2008-12-11 | Adeka Corp | Lubricant and grease base oil |
JP2009114354A (en) * | 2007-11-07 | 2009-05-28 | Kyodo Yushi Co Ltd | Grease composition |
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CN102471722A (en) | 2012-05-23 |
KR20120028976A (en) | 2012-03-23 |
WO2011016580A1 (en) | 2011-02-10 |
JP2011037950A (en) | 2011-02-24 |
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