JP5213215B2 - Lubricant composition and lubrication system using the same - Google Patents

Lubricant composition and lubrication system using the same Download PDF

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JP5213215B2
JP5213215B2 JP2007083799A JP2007083799A JP5213215B2 JP 5213215 B2 JP5213215 B2 JP 5213215B2 JP 2007083799 A JP2007083799 A JP 2007083799A JP 2007083799 A JP2007083799 A JP 2007083799A JP 5213215 B2 JP5213215 B2 JP 5213215B2
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lubricant composition
oil
amide
semi
acid amide
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JP2008239840A (en
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裕治 設楽
貴 開米
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Eneos Corp
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JXTG Nippon Oil and Energy Corp
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Priority to KR1020080028329A priority patent/KR101442256B1/en
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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
    • C10M169/04—Mixtures of base-materials 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
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
    • 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
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/02—Well-defined hydrocarbons
    • 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
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/22—Compounds 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
    • C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/16—Amides; Imides
    • 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

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Lubricants (AREA)

Description

本発明は、常温で半固体状の潤滑剤組成物に関し、特には、耐摩耗性や極圧性に優れるとともに、高い動摩擦係数を有する潤滑剤組成物に関する。本発明はさらに該潤滑剤組成物を伝動要素機構に用いた潤滑システムに関する。   The present invention relates to a lubricant composition that is semi-solid at room temperature, and particularly relates to a lubricant composition that is excellent in wear resistance and extreme pressure properties and has a high dynamic friction coefficient. The present invention further relates to a lubrication system using the lubricant composition in a transmission element mechanism.

近年、様々な産業技術において多機能化、高性能化、環境対応、省エネルギー、ロングライフ化が重要なキーテクノロジーとなっている。環境課題としては、二酸化炭素排出量の削減、省電力、省エネルギー、資源の有効活用など多々挙げることができる。そのため小型精密機械、産業機械、輸送システムなどの各種機械システムでは、環境に優しい工夫が施されるとともに、よりロングライフ化、信頼性の向上、高性能化などの特性が付与されるようになってきた。   In recent years, multi-functionality, high performance, environmental friendliness, energy saving, and long life have become important key technologies in various industrial technologies. There are many environmental issues such as reduction of carbon dioxide emissions, power saving, energy saving, and effective use of resources. For this reason, various mechanical systems such as small precision machines, industrial machines, and transportation systems have been devised to be environmentally friendly, and have been given characteristics such as longer life, improved reliability, and higher performance. I came.

ロングライフ化の一例として、機械の摺動部の潤滑性能を製品ライフまで不具合なく維持することが求められている。最近、機械システムの潤滑条件はより一層厳しくなっており、潤滑油剤には、より高性能な潤滑性が必要となっている。潤滑油剤には、液状の潤滑油と半固体状のグリースがあり、適宜用途に応じて使い分けられている。   As an example of extending the life, it is required to maintain the lubrication performance of the sliding portion of the machine without a problem until the product life. Recently, the lubrication conditions of mechanical systems have become more severe, and lubricating oils require higher performance lubricity. Lubricants include liquid lubricants and semi-solid greases, which are properly used depending on the application.

情報機器の普及がますます広まっている。携帯電話やノート型パソコンも様々なデザインが製品化されている。これらの製品では、ディスプレイ面と操作部が開閉式になっているものがあり、その開閉は、ヒンジと呼ばれる蝶番部品によって行われ、開閉の始動時にはスムーズに動くためにスティックスリップを抑制する観点から静摩擦係数と動摩擦係数の差ができるだけ小さい必要があり、また機器の使用中は、所望の開閉角度を長時間保つ必要があるため静摩擦係数ができるだけ高い必要がある。このようなヒンジは消費者に直接接する環境で使用されることが多いために油漏れによる汚染を徹底的に回避する必要があり、液状の潤滑油を適用することが困難であった。一方、グリースは常温では油漏れを抑制できるものの、摺動部の温度上昇により油分と増ちょう剤が分離すると油漏れを引き起こし、初期の潤滑性能が維持できない課題があった。ヒンジ以外に油剤の高い動力伝達能力が求められる伝動要素機構としては、ギヤ、ベルト、チェーン、ワイヤーロープ、機械式無段変速機などが挙げられる。このような要素機構は、家庭電化製品、ＯＡ機器、精密機械、工作機械などの各種産業機械、自動車、自動二輪車、自転車、鉄道などの輸送システムに幅広く用いられている。特に、機械式無段変速機には、高い動摩擦係数、トラクション係数が求められている。   The spread of information equipment is becoming increasingly widespread. Various designs of mobile phones and notebook computers have been commercialized. Some of these products have an openable and closable display surface and operation unit. The opening and closing is performed by a hinge part called a hinge. The difference between the coefficient of static friction and the coefficient of dynamic friction needs to be as small as possible, and the desired opening / closing angle must be maintained for a long time during use of the device, so that the coefficient of static friction needs to be as high as possible. Since such a hinge is often used in an environment in direct contact with consumers, it is necessary to thoroughly avoid contamination due to oil leakage, and it has been difficult to apply liquid lubricant. On the other hand, although grease can suppress oil leakage at normal temperature, there is a problem that if the oil component and the thickener are separated due to the temperature rise of the sliding portion, oil leakage occurs and the initial lubrication performance cannot be maintained. In addition to hinges, examples of transmission element mechanisms that require a high power transmission capability of oil include gears, belts, chains, wire ropes, and mechanical continuously variable transmissions. Such element mechanisms are widely used in various industrial machines such as home appliances, office automation equipment, precision machines, machine tools, and transportation systems such as automobiles, motorcycles, bicycles, and railways. In particular, a mechanical continuously variable transmission is required to have a high dynamic friction coefficient and traction coefficient.

これら伝動要素機構には、十分な潤滑性を有するとともに、高い動摩擦係数、トラクション係数が必要である。高い動摩擦係数を実現するためには、従来ナフテン系基油、シリコーン系基油が適用されてきた。これら基油に酸化防止剤、摩耗防止剤などが配合され、いわゆるトラクション油として使用されてきた。しかしトラクション油は、液状であるが故、油中に酸素がとけ込むので酸化劣化したり、温度上昇により蒸発したり、シール部から漏洩したりするなど機械システムのロングライフ化に際しての課題となっている。一方、グリースは、潤滑油を使用する場合に比べシステムを密閉構造にしなくとも良いが、高温では油分と増ちょう剤が分離し一度分離した油分と増ちょう剤は回復することはなく、摺動部が油剤不足になって初期性能が発揮されなくなったり、分離した油分が周辺を汚損する危険がある。   These transmission element mechanisms are required to have sufficient lubricity and a high dynamic friction coefficient and traction coefficient. In order to realize a high dynamic friction coefficient, naphthenic base oils and silicone base oils have been conventionally applied. These base oils are blended with antioxidants, antiwear agents and the like, and have been used as so-called traction oils. However, since traction oil is in liquid form, oxygen dissolves in the oil, which causes oxidation degradation, evaporation due to temperature rise, and leakage from the seal part. Yes. On the other hand, grease does not need to have a sealed structure as compared with the case of using lubricating oil, but at high temperatures, the oil and thickener are separated, and once separated, the oil and thickener will not recover and slide. There is a risk that the part will become insufficient in oil and the initial performance will not be exhibited, or the separated oil will contaminate the surroundings.

特に近年、機械システムの高機能化、小型化、長寿命化が強く求められており、潤滑剤にはより一層の高性能化、特には、極少量の油量でも不具合なく潤滑することが求められている。
これらの、課題に対し、本発明者は、熱可逆性ゲル状の潤滑性を有する組成物及び軸受用潤滑剤及びこれらを用いた軸受システムを提案している（特許文献２）が、ノート型パソコンや携帯電話器のヒンジ及び機械式無段変速機などの伝動要素機構に対して高い動摩擦係数と優れた耐摩耗性を示す潤滑剤を熱望する動きには依然根強いものがある。
特許第３７７５９８６号 国際特許公開 ＷＯ２００６―０５１６７１号 （社）日本トライボロジー学会編、トライボロジーハンドブック、養賢堂発行、（２００１）Ｐ２４７． In particular, in recent years, there has been a strong demand for higher performance, smaller size, and longer life of mechanical systems. Lubricants are required to have even higher performance, especially lubrication without problems even with extremely small amounts of oil. It has been.
In response to these problems, the present inventor has proposed a thermoreversible gel-like lubricating composition, a bearing lubricant, and a bearing system using these compositions (Patent Document 2). There is still a long-lasting movement that aspires for a lubricant that exhibits a high coefficient of dynamic friction and excellent wear resistance for transmission element mechanisms such as hinges of personal computers and mobile phones and mechanical continuously variable transmissions.
Japanese Patent No. 3775986 International Patent Publication WO 2006-056771 (Japan) Tribology Society of Japan, Tribology Handbook, published by Yokendo, (2001) P247.

本発明は上記課題を解決するもので、本発明は、極少量の油剤を潤滑摺動部に塗布し、薄膜状態においても高い潤滑性を有するとともに、動力伝達に有利な高い動摩擦係数を示す常温で半固体状の潤滑剤組成物を提供することを課題とし、さらにこの潤滑剤組成物を伝動要素機構に用いた潤滑システムを提供することを課題とする。   The present invention solves the above-mentioned problems, and the present invention applies a very small amount of an oil to a lubricated sliding portion, has a high lubricity even in a thin film state, and exhibits a high dynamic friction coefficient advantageous for power transmission. It is an object of the present invention to provide a semi-solid lubricant composition, and to provide a lubrication system using the lubricant composition in a transmission element mechanism.

本発明者らは、前記の課題を解決すべく、潤滑油基油、潤滑性を保持する化学物質、添加剤等について、及びそれらの組み合わせについて鋭意研究を進めた結果、本発明に想到した。   In order to solve the above-mentioned problems, the inventors of the present invention have arrived at the present invention as a result of diligent research on a lubricating base oil, chemical substances that retain lubricity, additives, and the like, and combinations thereof.

すなわち、本発明は、次のとおりの潤滑剤組成物及び潤滑システムである。
（１）％Ｃｐが７０以下である炭化水素基油、リン酸エステル、及びシリコーンから選択される少なくとも１種である液状基油を１０〜９８．９質量％、アルカリ土類金属塩を１〜２０質量％、及びアミド化合物を０．１〜８９質量％含み、常温で半固体状であることを特徴とする潤滑剤組成物。 That is, the present invention is the following lubricant composition and lubrication system.
(1) 10 to 98.9% by mass of a liquid base oil that is at least one selected from hydrocarbon base oils having a% Cp of 70 or less, phosphate esters, and silicones, and 1 to 1 alkaline earth metal salts A lubricant composition comprising 20% by mass and 0.1 to 89% by mass of an amide compound and being semisolid at normal temperature.

（２）アルカリ土類金属塩が、全塩基価が５〜４００ｍｇＫＯＨ／ｇであるスルホネート塩、フィネート塩、サリシレート塩から選択される少なくとも１種以上である（１）に記載の潤滑剤組成物。 (2) The lubricant composition according to (1), wherein the alkaline earth metal salt is at least one selected from a sulfonate salt, a finate salt, and a salicylate salt having a total base number of 5 to 400 mgKOH / g.

（３）アミド化合物が、下記の一般式（１）〜（３）で表される少なくとも1種の化合物である前述（１）又は（２）に記載の潤滑剤組成物、
式（１）〜（３）において、Ｒ１、Ｒ２、Ｒ３、Ｒ４、Ｒ５及びＲ６は、それぞれ独立して、炭素数５〜２５の飽和又は不飽和の鎖状炭化水素基であり、Ｒ２は水素であってもよい、Ａ１及びＡ２は、炭素数１〜１０のアルキレン基、フェニレン基、又は炭素数７〜１０のアルキルフェニレン基から選択される炭素数１〜１０の２価の炭化水素基である。
（４）一般式（１）〜（３）で表されるアミド化合物は、Ｒ１、Ｒ２、Ｒ３、Ｒ４、Ｒ５及びＲ６が、それぞれ独立して炭素数１２〜２０の飽和鎖状炭化水素基を有する、又はＲ２は水素であるアミド化合物及び／又はＲ１とＲ２、Ｒ３とＲ４、及びＲ５とＲ６の少なくともいずれか一方が炭素数１２〜２０の不飽和鎖状炭化水素基を有するアミド化合物である（３）に記載の潤滑剤組成物。 (3) The lubricant composition according to the above (1) or (2), wherein the amide compound is at least one compound represented by the following general formulas (1) to (3):
In the formulas (1) to (3), R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are each independently a saturated or unsaturated chain hydrocarbon group having 5 to 25 carbon atoms. And R 2 may be hydrogen. A 1 and A 2 are selected from an alkylene group having 1 to 10 carbon atoms, a phenylene group, or an alkylphenylene group having 7 to 10 carbon atoms. 10 is a divalent hydrocarbon group.
(4) In the amide compounds represented by the general formulas (1) to (3), R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are each independently saturated with 12 to 20 carbon atoms. An amide compound having a chain hydrocarbon group or R 2 is hydrogen and / or at least one of R 1 and R 2 , R 3 and R 4 , and R 5 and R 6 has 12 to 20 carbon atoms The lubricant composition according to (3), which is an amide compound having an unsaturated chain hydrocarbon group.

（５）（１）〜（４）のいずれかに記載の潤滑剤組成物を伝動要素機構に用いたことを特徴とする潤滑システム。
（６）伝動要素機構として、特には、所定の角度保持が求められるヒンジ、トラクション係数が高い油剤によって動力伝達を行う機械式無段変速機などが挙げられる。 (5) A lubrication system using the lubricant composition according to any one of (1) to (4) in a transmission element mechanism.
(6) Examples of the transmission element mechanism include a hinge that is required to maintain a predetermined angle, and a mechanical continuously variable transmission that transmits power using an oil having a high traction coefficient.

本発明の潤滑剤組成物によれば、潤滑摺動部に少量塗布することにより、摺動時において安定した薄膜を形成し、高い極圧性と高い動摩擦係数を示すという格別の効果を奏する。また、本発明の潤滑剤組成物は、熱可逆性を有し、常温では半固体状を示し、アミド化合物の融点以上の温度では均一液体状態を示すものであるから、摺動部では加熱−冷却で液体−半固体を繰り返し、摺動部から離れて温度が融点以上に上がらないところでは半固体を保つことができる。そのため酸化劣化、蒸発消失、油漏れすることはなく、ギヤ、ベルト、チェーン、ワイヤーロープ、ヒンジ、機械式無段変速機などの伝動要素機構の潤滑剤として有効に用いることができる。   According to the lubricant composition of the present invention, by applying a small amount to the lubrication sliding portion, a stable thin film is formed at the time of sliding, and there is an extraordinary effect of exhibiting high extreme pressure properties and a high dynamic friction coefficient. Further, the lubricant composition of the present invention has thermoreversibility, exhibits a semi-solid state at room temperature, and exhibits a uniform liquid state at a temperature equal to or higher than the melting point of the amide compound. The liquid-semi-solid is repeated by cooling, and the semi-solid can be maintained where the temperature does not rise above the melting point away from the sliding part. Therefore, there is no oxidative deterioration, evaporation disappearance, or oil leakage, and it can be effectively used as a lubricant for transmission element mechanisms such as gears, belts, chains, wire ropes, hinges, and mechanical continuously variable transmissions.

本発明は、液状基油を１０〜９８．９質量％、金属塩を１〜２０質量％、及びアミド化合物を０．１〜８９質量％含み、常温で半固体状であることを特徴とする潤滑剤組成物であり、潤滑を要する伝動要素機構に塗布しておくと、潤滑を要する状態になったとき、液状となって高い動摩擦係数を発揮する。特に、焼付トラブルが心配される低速、高荷重のサービスなど、極圧潤滑が要求されるサービスに有用であり、薄膜下で高い潤滑性を示すとともに、油保特性にも優れているため油切れが生じにくいことから焼付が起こりにくくなる。また、本発明の潤滑剤組成物は、伝動要素機構の摺動部が運動を始めると当該摺動部の温度が上昇し、半固体状から液体状態になり狭い摺動部に進入して潤滑剤組成物として働くが、摺動部から離れて摩擦熱が伝播しない部分は半固体の状態を保持するため、いわゆるオイル漏れを心配する必要がなく、周囲を常時清潔に保つことができる。
なお、ここで「常温」とは室内の普通の温度を意味し、具体的には、−２０〜５０℃、より一般的には−１０〜３０℃程度の温度環境をいう。
該潤滑剤組成物は、高い動摩擦係数が得られ、例えば、０．１〜０．３、特には０．１４〜０．２０、更には０．１５〜０．１８を示すものが好ましい。 The present invention is characterized by containing 10 to 98.9% by mass of a liquid base oil, 1 to 20% by mass of a metal salt, and 0.1 to 89% by mass of an amide compound, and being semi-solid at room temperature. When the lubricant composition is applied to a transmission element mechanism requiring lubrication, it becomes liquid and exhibits a high coefficient of dynamic friction when it is in a state requiring lubrication. It is particularly useful for services that require extreme pressure lubrication, such as low-speed and high-load services where there are concerns about seizure problems, and it exhibits high lubricity under thin films and has excellent oil retention characteristics. Since seizure hardly occurs, seizure hardly occurs. In addition, the lubricant composition of the present invention, when the sliding portion of the transmission element mechanism starts to move, the temperature of the sliding portion rises, changes from a semi-solid state to a liquid state, enters the narrow sliding portion, and lubricates. Although it works as an agent composition, the part where the frictional heat does not propagate away from the sliding part maintains a semi-solid state, so there is no need to worry about so-called oil leakage, and the surroundings can always be kept clean.
Here, “normal temperature” means a normal temperature in the room, specifically, a temperature environment of about −20 to 50 ° C., more generally about −10 to 30 ° C.
The lubricant composition has a high coefficient of dynamic friction, and is preferably 0.1 to 0.3, particularly 0.14 to 0.20, and more preferably 0.15 to 0.18.

［液状基油］
本発明に用いる液状基油は、％Ｃｐが７０以下である炭化水素基油、リン酸エステル、及びシリコーンから選択される少なくとも１種である。炭化水素基油、リン酸エステル、及びシリコーンは単独または２種以上の混合油として用いることができる。
％Ｃｐが７０以下である炭化水素基油としては、アルキルナフテン、アルキルベンゼンが好ましく用いられ、鉱油基油を用いることもできる。炭化水素基油は、炭化水素化合物からなり、ナフテン、アロマの環状の炭化水素を多く含むこと、すなわち、％Ｃｎと％Ｃａの和が３０を超えることが必要である。炭化水素基油の粘度指数は、８０以下が、特には２０以下が好ましく、通常は−４００以上である。液状基油の物性は、特に限定するものではないが、好ましくは４０℃における動粘度が５〜５０００ｍｍ２／ｓ、より好ましく５０〜３０００ｍｍ２／ｓ、更に好ましくは５００〜２０００ｍｍ２／ｓである。なお、％Ｃａ、％Ｃｐ及び％Ｃｎは、ＡＳＴＭ Ｄ３２３８に規定されるｎ-ｄ-Ｍ環分析によって求められるものである。 [Liquid base oil]
The liquid base oil used in the present invention is at least one selected from hydrocarbon base oils having a% Cp of 70 or less, phosphate esters, and silicones. The hydrocarbon base oil, phosphate ester, and silicone can be used alone or as a mixture of two or more.
Alkyl naphthene and alkyl benzene are preferably used as the hydrocarbon base oil having a% Cp of 70 or less, and a mineral oil base oil can also be used. The hydrocarbon base oil is composed of a hydrocarbon compound and contains a large amount of cyclic hydrocarbons of naphthene and aroma, that is, the sum of% Cn and% Ca needs to exceed 30. The viscosity index of the hydrocarbon base oil is preferably 80 or less, particularly preferably 20 or less, and usually −400 or more. Physical properties of the liquid base oil is not particularly limited, is preferably a kinematic viscosity of 5 to 5000 mm 2 / s at 40 ° C., more preferably 50~3000mm 2 / s, more preferably 500~2000mm 2 / s . Note that% Ca,% Cp, and% Cn are determined by the ndM ring analysis defined in ASTM D3238.

アルキルナフテンとしては、合成ナフテン、ナフテン系鉱油がある。アルキルベンゼンとしては、合成系ハードアルキルベンゼン、ソフトアルキルベンゼンがある。リン酸エステルとしては、正リン酸エステル、亜リン酸エステルなどがあるが、一般的にはトリクレジルホスフェートなどが挙げられる。シリコーン系油としては、ポリジメチルシロキサン、ポリメチルフェニルシロキサンなどがその一例として挙げられる。   Alkyl naphthenes include synthetic naphthenes and naphthenic mineral oils. Alkylbenzene includes synthetic hard alkylbenzene and soft alkylbenzene. Examples of phosphoric acid esters include orthophosphoric acid esters and phosphorous acid esters, and generally include tricresyl phosphate. Examples of the silicone oil include polydimethylsiloxane and polymethylphenylsiloxane.

なかでも、％Ｃａが１０以下である炭化水素基油、具体的には、アルキルナフテンが、高い動摩擦特性、潤滑性の面で優れており、好ましく用いることができる。これらの基油は、上記の物性を満足するのであれば、単独で用いることもできるし、２種以上を組み合わせて用いることもできる。
液状基油は、仕上がりの常温で半固体状である潤滑剤組成物に１０〜９８．９質量％、好ましくは３０〜９７質量％、更に好ましくは７０〜９３質量％含まれるよう配合する。液状基油の配合量が、この範囲未満では、基油としての高い動摩擦特性が得られず好ましくない。 Among these, hydrocarbon base oils having a% Ca of 10 or less, specifically, alkyl naphthenes are excellent in terms of high dynamic friction characteristics and lubricity, and can be preferably used. These base oils can be used alone or in combination of two or more as long as the above physical properties are satisfied.
The liquid base oil is blended so that it is contained in the finished lubricant composition that is semi-solid at a normal temperature of 10 to 98.9% by mass, preferably 30 to 97% by mass, and more preferably 70 to 93% by mass. When the blending amount of the liquid base oil is less than this range, it is not preferable because high dynamic friction characteristics as a base oil cannot be obtained.

［アルカリ土類金属塩］
本発明には、動摩擦係数を高めるため、Ｃａ、Ｂａ、Ｍｇなどのアルカリ土類金属塩、好ましくは、アルカリ土類金属の有機酸塩を用いる。有機酸としては、カルボン酸、スルホン酸、フェノール、ホスホン酸、サリチル酸などを用いることができる。なかでも、スルホネート塩、フィネート塩、サリシレート塩から選択される少なくとも１種以上のアルカリ土類金属塩か好ましく、さらに、Ｃａのアルカリ土類金属のスルホネート、フィネート、サリシレートなどを、特にはスルホネートを好ましく用いることができる。これらは、金属系清浄分散剤として市販されている。これらアルカリ土類金属塩は、炭酸塩からなる過塩基成分が含まれていても良く、具体的には全塩基価が５〜４００ｍｇＫＯＨ／ｇ、特には５０〜４００ｍｇＫＯＨ／ｇであるアルカリ土類金属塩がより好ましく用いることができる。
アルカリ土類金属塩は、仕上がりの常温で半固体状である潤滑剤組成物に１〜２０質量％、好ましくは２〜２０質量％、更に好ましくは２〜１０質量％含まれるよう配合する。金属塩の配合量が、この範囲未満では、摩擦特性への効果的な寄与が得られず、一方、この範囲を超えて配合しても摩擦特性への寄与効果が頭打ちとなりコスト高になるため、好ましくない。 [Alkaline earth metal salts]
In the present invention, alkaline earth metal salts such as Ca, Ba and Mg, preferably organic acid salts of alkaline earth metals are used in order to increase the dynamic friction coefficient. As the organic acid, carboxylic acid, sulfonic acid, phenol, phosphonic acid, salicylic acid and the like can be used. Among them, at least one alkaline earth metal salt selected from sulfonate salts, finate salts, and salicylate salts is preferable, and Ca alkaline earth metal sulfonates, finates, salicylates, and the like are preferable, and sulfonates are particularly preferable. Can be used. These are commercially available as metallic detergents and dispersants. These alkaline earth metal salts may contain an overbase component made of carbonate, specifically, an alkaline earth metal having a total base number of 5 to 400 mgKOH / g, particularly 50 to 400 mgKOH / g. A salt can be used more preferably.
The alkaline earth metal salt is blended so as to be contained in the lubricant composition that is semi-solid at the finished normal temperature so as to be contained in an amount of 1 to 20% by mass, preferably 2 to 20% by mass, and more preferably 2 to 10% by mass. If the blending amount of the metal salt is less than this range, an effective contribution to the friction characteristics cannot be obtained. On the other hand, if the blending amount exceeds this range, the contribution effect to the friction characteristics reaches its peak and the cost increases. It is not preferable.

［アミド化合物］
本発明に用いるアミド化合物は、アミド基（−ＮＨ−ＣＯ−）を１つ以上有する脂肪酸アミド化合物であり、次の式（１）で表されるアミド基が１個のモノアミド、及び式（２）及び（３）で表されるアミド基を２個有するビスアミドを好ましく用いることができる。モノアミドとビスアミドを組み合わせて用いることが好ましい。

式中、Ｒ１及びＲ２は、それぞれ独立して、炭素数５〜２５の飽和又は不飽和の鎖状炭化水素基であり、さらに、Ｒ２は水素であってもよい。

式（２）及び（３）において、Ｒ３、Ｒ４、Ｒ５及びＲ６は、それぞれ独立して、炭素数５〜２５の飽和又は不飽和の鎖状炭化水素基であり、Ａ１及びＡ２は、炭素数１〜１０のアルキレン基、フェニレン基又は炭素数７〜１０のアルキルフェニレン基から選択される炭素数１〜１０の２価の炭化水素基である。なお、アルキルフェニレン基の場合、フェニレン基とアルキル基及び／又はアルキレン基の２個以上とが結合したかたちの２価の炭化水素基であってもよい。 [Amide compound]
The amide compound used in the present invention is a fatty acid amide compound having one or more amide groups (—NH—CO—), a monoamide having one amide group represented by the following formula (1), and the formula (2 ) And bisamide having two amide groups represented by (3) can be preferably used. It is preferable to use a combination of monoamide and bisamide.

In the formula, R 1 and R 2 are each independently a saturated or unsaturated chain hydrocarbon group having 5 to 25 carbon atoms, and R 2 may be hydrogen.

In the formulas (2) and (3), R 3 , R 4 , R 5 and R 6 are each independently a saturated or unsaturated chain hydrocarbon group having 5 to 25 carbon atoms, and A 1 and a 2 is a divalent hydrocarbon group having 1 to 10 carbon atoms selected from an alkylene group, an alkyl phenylene group having a phenylene group or a 7 to 10 carbon atoms having 1 to 10 carbon atoms. In the case of an alkylphenylene group, it may be a divalent hydrocarbon group in which two or more of a phenylene group and an alkyl group and / or an alkylene group are bonded.

モノアミド化合物は、上記式（１）で表されるが、Ｒ１及びＲ２を構成する水素の一部は水酸基で置換されていてもよい。このようなモノアミド化合物として、具体的には、ラウリン酸アミド、パルミチン酸アミド、ステアリン酸アミド、ベヘン酸アミド、ヒドロキシステアリン酸アミド等の飽和脂肪酸アミド、オレイン酸アミド、エルカ酸アミドなどの不飽和脂肪酸アミド、及びステアリルステアリン酸アミド、オレイルオレイン酸アミド、オレイルステアリン酸アミド、ステアリルオレイン酸アミド等の飽和又は不飽和の長鎖脂肪酸と長鎖アミンによる置換アミド類などが挙げられる。 The monoamide compound is represented by the above formula (1), but a part of hydrogen constituting R 1 and R 2 may be substituted with a hydroxyl group. Specific examples of such monoamide compounds include saturated fatty acid amides such as lauric acid amide, palmitic acid amide, stearic acid amide, behenic acid amide, and hydroxystearic acid amide, and unsaturated fatty acids such as oleic acid amide and erucic acid amide. Examples thereof include amides, and substituted amides with saturated or unsaturated long-chain fatty acids and long-chain amines such as stearyl stearamide, oleyl oleate, oleyl stearate, stearyl oleamide, and the like.

これらのモノアミド化合物の中でも、式（１）のＲ１及びＲ２がそれぞれ独立して炭素数１２〜２０の飽和鎖状炭化水素基のアミド化合物及び／又はＲ１とＲ２の少なくともいずれか一方が炭素数１２〜２０の不飽和鎖状炭化水素基のアミド化合物であることが好ましく、両アミド化合物の混合物がより好ましい。さらに不飽和鎖状炭化水素基が炭素数１８の不飽和結合を有するオレイル基であるモノアミド化合物が好ましい。具体的にはオレイン酸アミド、オレイルオレイン酸アミドが好ましく、摺動部に薄膜を形成し、保持し、焼付トラブルの解消に効果的な薄膜保持性を確保する。 Among these monoamide compounds, R 1 and R 2 in the formula (1) are each independently an amide compound having a saturated chain hydrocarbon group having 12 to 20 carbon atoms and / or at least one of R 1 and R 2. Is preferably an amide compound of an unsaturated chain hydrocarbon group having 12 to 20 carbon atoms, and more preferably a mixture of both amide compounds. Furthermore, a monoamide compound in which the unsaturated chain hydrocarbon group is an oleyl group having an unsaturated bond having 18 carbon atoms is preferred. Specifically, oleic acid amide and oleyl oleic acid amide are preferable, and a thin film is formed and held on the sliding portion, and the thin film retainability effective in solving the seizure trouble is ensured.

ビスアミド化合物としては、ジアミンの酸アミド又はジ酸の酸アミドのかたちをした上記式（２）又は（３）でそれぞれ表される化合物である。なお、式（２）及び（３）でＲ３、Ｒ４、Ｒ５及びＲ６、さらにＡ１及びＡ２で表される炭化水素基において、一部の水素が水酸基（−ＯＨ）で置換されていてもよい。
式（２）で表されるアミド化合物として、具体的には、エチレンビスステアリン酸アミド、エチレンビスイソステアリン酸アミド、エチレンビスオレイン酸アミド、メチレンビスラウリン酸アミド、ヘキサメチレンビスオレイン酸アミド、ヘキサメチレンビスヒドロキシステアリン酸アミド、ｍ−キシリレンビスステアリン酸アミド等が挙げられる。式（３）で表されるアミド化合物として、具体的には、Ｎ,Ｎ’−ジステアリルセバシン酸アミドなどが挙げられる。 The bisamide compound is a compound represented by the above formula (2) or (3) in the form of a diamine acid amide or a diacid acid amide. In addition, in the hydrocarbon groups represented by R 3 , R 4 , R 5 and R 6 , and A 1 and A 2 in the formulas (2) and (3), some hydrogens are substituted with hydroxyl groups (—OH). May be.
Specific examples of the amide compound represented by the formula (2) include ethylene bis stearic acid amide, ethylene bis isostearic acid amide, ethylene bis oleic acid amide, methylene bis lauric acid amide, hexamethylene bis oleic acid amide, and hexamethylene. Examples thereof include bishydroxystearic acid amide and m-xylylene bisstearic acid amide. Specific examples of the amide compound represented by the formula (3) include N, N′-distearyl sebacic acid amide.

これらビスアミド化合物の中でも、モノアミド化合物の場合と同様に、式（２）のＲ３とＲ４及び式（３）のＲ５とＲ６がそれぞれ独立して炭素数１２〜２０の飽和鎖状炭化水素基のアミド化合物及び／又はＲ３とＲ４及びＲ５とＲ６の少なくともいずれか一方が炭素数１２〜２０の不飽和鎖状炭化水素基のアミド化合物であることが好ましく、両アミド化合物の混合物がより好ましい。さらに不飽和鎖状炭化水素基が炭素数１８の不飽和結合を有するオレイル基であるビスアミド化合物が薄膜保持性を確保する上で好ましい。このような化合物として、エチレンビスオレイン酸アミド、ヘキサメチレンビスオレイン酸アミドなどが挙げられる。 Among these bisamide compounds, as in the case of the monoamide compound, R 3 and R 4 in the formula (2) and R 5 and R 6 in the formula (3) are each independently a saturated chain carbonization having 12 to 20 carbon atoms. Preferably, the amide compound of a hydrogen group and / or at least one of R 3 and R 4 and R 5 and R 6 is an amide compound of an unsaturated chain hydrocarbon group having 12 to 20 carbon atoms, both amide compounds The mixture of is more preferable. Further, a bisamide compound in which the unsaturated chain hydrocarbon group is an oleyl group having an unsaturated bond having 18 carbon atoms is preferable for ensuring thin film retention. Examples of such compounds include ethylene bisoleic acid amide and hexamethylene bisoleic acid amide.

アミド化合物は、液状基油と均一に混合すると、常温でゲル状の潤滑性を有する組成物を形成する。したがって、アミド化合物は、液状基油を半固体状化（ゲル化）する半固体状化化合物として働くとともに、潤滑剤組成物本来の潤滑特性を発揮する状況においては、摩擦熱で融解して液体の潤滑剤組成物として働くことになる。常温で半固体、高温で液体の状態で使用されることを考えると、好ましく用いられるアミド化合物としては、融点は５０〜２００℃が好ましく、より好ましくは８０〜１８０℃であり、さらに分子量は１００〜１０００が好ましく、より好ましくは１５０〜８００である。   When the amide compound is uniformly mixed with the liquid base oil, it forms a gel-like composition at room temperature. Therefore, the amide compound works as a semi-solid compound that makes the liquid base oil semi-solid (gelled), and in a situation where the lubricant composition exhibits the inherent lubricating properties, it melts by frictional heat and becomes a liquid. It will work as a lubricant composition. Considering that it is used in a semi-solid state at normal temperature and in a liquid state at high temperature, the amide compound preferably used has a melting point of preferably 50 to 200 ° C., more preferably 80 to 180 ° C., and a molecular weight of 100. -1000 is preferable, More preferably, it is 150-800.

また機械システムの設計上の制約から極少量の油剤しか用いることができない摺動部で厳しい潤滑環境下においても焼付きなどを起こさないためには、摺動表面に油剤が強固に吸着・付着し、油膜を保持しなければならない。そのためには付着性を有する油剤が必要であるが、本発明では、半固体状化化合物であるアミド化合物の炭化水素基が不飽和鎖状であると付着性が増すことを見出した。付着性が増すと摺動表面へ薄膜状に塗布することができ、厳しい潤滑環境においても油膜切れを起こしにくくなり、潤滑性能が向上する。不飽和鎖状炭化水素基としては、炭素数１８の不飽和結合を有するオレイル基であるビスアミド化合物が好ましい。
アミド化合物は、仕上がりの常温で半固体状である潤滑剤組成物に０．１〜９０質量％、好ましくは１〜５０質量％、更に好ましくは５〜２０質量含まれるように配合する。アミド化合物の配合量が、この範囲未満では、常温でゲル状の組成物を形成することができず、一方、この範囲を超えて配合しても硬くなり過ぎてハンドリングしにくく、好ましくない。 In order to prevent seizure in a severe lubrication environment at sliding parts where only a small amount of oil can be used due to mechanical system design restrictions, the oil adheres firmly to the sliding surface. Must hold the oil film. For this purpose, an oil agent having adhesiveness is required. However, in the present invention, it has been found that the adhesiveness increases when the hydrocarbon group of the amide compound, which is a semi-solidified compound, is an unsaturated chain. When the adhesion increases, it can be applied to the sliding surface in a thin film, and it becomes difficult to cause an oil film breakage even in a severe lubrication environment, and the lubrication performance is improved. As the unsaturated chain hydrocarbon group, a bisamide compound which is an oleyl group having an unsaturated bond having 18 carbon atoms is preferable.
The amide compound is blended so as to be contained in the finished lubricant composition that is semi-solid at normal temperature in an amount of 0.1 to 90% by mass, preferably 1 to 50% by mass, and more preferably 5 to 20% by mass. If the blending amount of the amide compound is less than this range, a gel-like composition cannot be formed at room temperature.

［潤滑剤組成物の調製］
本発明の常温で半固体状である潤滑剤組成物は、特に限定するものではないが、液状基油、金属塩及びアミド化合物を上記の配合割合で均一に混合することによって調製することができる。例えば、液状基油、金属塩、アミド化合物をそれぞれ所定量計り取り融点以上に加熱して液体状態で均一になるよう攪拌した後、冷却して半固体状にすることにより得ることができる。 [Preparation of Lubricant Composition]
The lubricant composition that is semi-solid at room temperature according to the present invention is not particularly limited, but can be prepared by uniformly mixing the liquid base oil, the metal salt, and the amide compound in the above-described blending ratio. . For example, it can be obtained by measuring a predetermined amount of each of the liquid base oil, the metal salt, and the amide compound, heating them to the melting point or higher and stirring them uniformly in the liquid state, and then cooling them to make them semisolid.

本発明の組成物には、さらに周知の極圧剤、腐食防止剤、摩耗防止剤、防錆剤、酸化防止剤、及び消泡剤などの添加剤を適宜配合することができる。極圧剤、摩耗防止剤としてジアルキルジチオリン酸亜鉛、硫黄系化合物、リン系化合物など、腐食防止剤としてのチアジアゾール誘導体、ベンゾトリアゾールおよびこの誘導体、防錆剤として脂肪酸部分エステル、リン系化合物など、酸化防止剤としてフェノール系、アミン系化合物など、及び消泡剤としてシリコーン系化合物、ＰＭＡポリマー、流動点降下剤、粘度指数向上剤としてＰＭＡポリマーなどが挙げられる。また、前記各種の添加剤は、数種が予め混合されたいわゆる添加剤パッケージの形で用いることもできる。   In the composition of the present invention, additives such as well-known extreme pressure agents, corrosion inhibitors, antiwear agents, rust inhibitors, antioxidants, and antifoaming agents can be appropriately blended. Extreme pressure agent, zinc dialkyldithiophosphate, sulfur compound, phosphorus compound as antiwear agent, thiadiazole derivative, benzotriazole and this derivative as corrosion inhibitor, fatty acid partial ester, phosphorus compound, etc. as rust inhibitor Examples of the inhibitor include phenolic compounds and amine compounds, and examples of the antifoaming agent include silicone compounds, PMA polymers, pour point depressants, and viscosity index improvers such as PMA polymers. The various additives can also be used in the form of a so-called additive package in which several kinds are mixed in advance.

本発明の常温で半固体状である潤滑剤組成物は、潤滑作用を要する機械機構（摺動部）に適用すると、摺動時には摩擦熱によって液体に状態を変え摺動部に浸透して、金属や樹脂などの摺動部を構成する固体の表面に薄膜を形成して摺動部を潤滑する。摺動が停止すれば、温度が低下し、液体状態であった潤滑剤組成物は再び半固体状（ゲル状）に戻る。また、本発明の潤滑剤組成物は、特に高焼付荷重、高い動摩擦係数を有し、さらにこの優れた摩擦特性を長期にわたって持続することから、用途としては低速、高荷重の極圧サービスに好適であり、また、潤滑剤の補給がしにくい摺動部や一旦組み立てたら開放することのない構造のデバイスの摺動部にも好適に用いることができる。さらに、本発明の潤滑剤組成物は、使用、不使用にともなう昇温、冷却ストレスを繰り返して受けてもゲル（半固体状）構造が再構築されるから、油漏れによる汚染を回避でき、蒸発しにくく、ロングライフである。
したがって従来の液状トラクション油の代替として十分使用でき、例えば、ギヤ、ベルト、チェーン、ワイヤーロープ、ヒンジ、機械式無段変速機などの伝動要素機構に、それも高負荷の伝動要素機構に好適に使用することができる。特に好ましい用途としては、所望の角度保持が求められる開閉式のラップトップパソコン、携帯電話や電子辞書などのヒンジ、動摩擦係数が高い潤滑剤によって動力伝達を行う機械式無段変速機などが挙げられる。 When applied to a mechanical mechanism (sliding part) that requires a lubricating action, the lubricant composition that is semi-solid at room temperature of the present invention changes its state to liquid by frictional heat during sliding and penetrates into the sliding part, A thin film is formed on the surface of the solid constituting the sliding part such as metal or resin to lubricate the sliding part. When the sliding stops, the temperature decreases, and the lubricant composition in the liquid state returns to a semi-solid state (gel state) again. In addition, the lubricant composition of the present invention has a particularly high seizure load and a high dynamic friction coefficient, and further maintains this excellent friction characteristic over a long period of time, so that it is suitable for low pressure and high load extreme pressure services. In addition, it can also be suitably used for a sliding portion where it is difficult to replenish the lubricant and a sliding portion of a device having a structure that does not open once assembled. Furthermore, the lubricant composition of the present invention can avoid contamination due to oil leakage because the gel (semi-solid state) structure is reconstructed even after repeated use of temperature rise and cooling stress associated with use and non-use. It is hard to evaporate and has a long life.
Therefore, it can be used satisfactorily as a substitute for conventional liquid traction oil, and is suitable for transmission element mechanisms such as gears, belts, chains, wire ropes, hinges, mechanical continuously variable transmissions, etc. Can be used. Particularly preferred applications include an open / close laptop computer that requires a desired angle hold, a hinge such as a mobile phone or an electronic dictionary, and a mechanical continuously variable transmission that transmits power using a lubricant having a high dynamic friction coefficient. .

以下に、実施例を用いて本発明をより詳しく説明するが、本発明はこれに限定されるものではない。   Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited thereto.

［液状基油］
実施例及び比較例用の潤滑剤組成物を調製するために次の３種類の液状基油を用いた。
基油Ａ：合成ナフテン（テクケム社製Ｔｅｃｈｔｒａｃ Ｍ３Ｃｏｎｃ）
基油Ｂ：ソフトアルキルベンゼン（動粘度（４０℃）：３２ｍｍ２／ｓ）
基油Ｃ：α−オレフィンオリゴマー（Ｍｏｂｉｌ社製ＳＨＦ−４００）
この３種類の液状基油の物性を表１に示す。なお、これらの液状基油には、酸化防止剤、摩耗防止剤などの添加剤があらかじめ所定量配合されており、潤滑油としての基本性能（酸化防止、摩耗防止など）を有している。 [Liquid base oil]
The following three types of liquid base oils were used to prepare lubricant compositions for Examples and Comparative Examples.
Base oil A: Synthetic naphthene (Techtrac M3Conc, manufactured by Techchem)
Base oil B: Soft alkylbenzene (kinematic viscosity (40 ° C.): 32 mm 2 / s)
Base oil C: α-olefin oligomer (Mobil SHF-400)
Table 1 shows the physical properties of these three types of liquid base oils. These liquid base oils are pre-mixed with predetermined amounts of additives such as antioxidants and antiwear agents, and have basic performance (such as antioxidation and wear prevention) as a lubricating oil.

［アミド化合物］
液状基油に配合し、半固体状化するために以下のアミド化合物を用いた。
アミドＡ：エチレンビスオレイン酸アミド（日本化成製、スリパックスＯ、融点１１９℃）
アミドＢ：エチレンビスステアリン酸アミド（日本化成製、スリパックスＥ、融点１４５℃） [Amide compound]
The following amide compounds were used for blending into a liquid base oil and making it semi-solid.
Amide A: Ethylene bisoleic acid amide (Nippon Kasei Chemicals, Sripacs O, melting point 119 ° C)
Amide B: Ethylene bis-stearic acid amide (Nippon Kasei, Sripacks E, melting point 145 ° C)

［アルカリ土類金属塩］
アルカリ土類金属塩としては次の２種類の化合物を用いた。
Ｃａスルホネート：全塩基価３００ｍｇＫＯＨ／ｇ
Ｃａサリシレート：全塩基価７０ｍｇＫＯＨ／ｇ [Alkaline earth metal salts]
The following two types of compounds were used as alkaline earth metal salts.
Ca sulfonate: Total base number 300 mgKOH / g
Ca salicylate: Total base number 70 mgKOH / g

［グリース］
本願発明の潤滑剤組成物と比較するため、比較例４として市販のリチウム（Ｌｉ）グリース（ジャパンエナジー製、リゾニックスグリースＮｏ．２、ちょう度番号２号（混和ちょう度範囲２６５〜２９５））を用いた。 [Grease]
In order to compare with the lubricant composition of the present invention, as Comparative Example 4, a commercially available lithium (Li) grease (manufactured by Japan Energy, Risonix Grease No. 2, consistency number 2 (mixing consistency range 265 to 295)) Was used.

［潤滑剤組成物の調製］
上記液状基油として基油Ａ（合成ナフテン）、基油Ｂ（アルキルベンゼン）、および基油Ｃ（α−オレフィンオリゴマー）を、アミド化合物としてアミドＡ（エチレンビスオレイン酸アミド）及びアミドＢ（エチレンビスステアリン酸アミド）を、そしてアルカリ土類金属塩としてＣａスルホネート及びＣａサリシレートを用いて実施例１〜６及び比較例３の供試油（潤滑剤組成物）を以下の手順で調製した。 [Preparation of Lubricant Composition]
Base oil A (synthetic naphthene), base oil B (alkylbenzene), and base oil C (α-olefin oligomer) are used as the liquid base oil, and amide A (ethylene bisoleic acid amide) and amide B (ethylene bis) are used as the amide compounds. Test oils (lubricant compositions) of Examples 1 to 6 and Comparative Example 3 were prepared by the following procedure using stearic acid amide) and Ca sulfonate and Ca salicylate as alkaline earth metal salts.

ステンレス製のビーカーに、液状基油、アルカリ土類金属塩、アミド化合物を表２の上部に示す仕上がり供試油に対する割合（質量％）で、それぞれ約１００ｍｌの供試油が得られるように所定量計り取り、卓上電磁ヒーターを用い、アミド化合物の融点以上（融点＋２０℃）に加温しながら撹拌した。均一に溶解したことを外観の観察で判断した後、均一溶解液を耐熱ガラス容器（内径６０ｍｍ×高さ９０ｍｍ）に約１００ｍｌを移し、放冷し、実施例１〜６及び比較例３の常温で半固体状の潤滑剤組成物をそれぞれ調製した。   Place the base oil, alkaline earth metal salt, and amide compound in a stainless steel beaker at a ratio (mass%) to the finished test oil shown in the upper part of Table 2 so that about 100 ml of the test oil can be obtained. Quantitatively measured and stirred using a desktop electromagnetic heater while heating to a temperature above the melting point of the amide compound (melting point + 20 ° C.). After judging the uniform dissolution by observing the appearance, about 100 ml of the uniform solution was transferred to a heat-resistant glass container (inner diameter 60 mm × height 90 mm), allowed to cool, and normal temperatures of Examples 1 to 6 and Comparative Example 3 A semi-solid lubricant composition was prepared.

なお、比較例１は、アミド化合物とアルカリ土類金属塩をともに含有しない、基油Ａの合成ナフテンのみからなる供試油であり、また、比較例２は、アミド化合物を含有せず、基油Ａの合成ナフテンと金属塩としてＣａスルホネートとからなる供試油であり、ともに常温で液体の潤滑性を有する組成物である。また、比較例４は、上記の市販Ｌｉグリースである。   In addition, Comparative Example 1 is a test oil made of only synthetic naphthene of base oil A, which contains neither an amide compound nor an alkaline earth metal salt, and Comparative Example 2 contains no amide compound, It is a test oil composed of synthetic naphthene of oil A and Ca sulfonate as a metal salt, both of which are liquid lubricating compositions at room temperature. Moreover, the comparative example 4 is said commercially available Li grease.

［評価方法］
実施例１〜６及び比較例１〜４の各潤滑剤組成物の評価試験（摩擦係数の測定など）を以下に記した方法に従って実施した。その結果を表２の下部に示す。
（１）ＳＲＶ試験
ＡＳＴＭ Ｄ５７０６に規定されているボールオンディスク型ＳＲＶ摩擦試験機を用いた。ボールは、材質がＳＵＪ−２の直径１０ｍｍのボールベアリング用鋼球を用い、またディスクは、材質がＳＵＪ−２の直径２４ｍｍ、厚さ７．８５ｍｍの円盤状の試験片を用いた。なお、ディスクの表面は粗さ（ＲＺ）が０．４５〜０．６５μｍであるラッピング仕上げを施した。摩擦試験は、荷重５０Ｎ、振幅数５０Ｈｚ、振幅幅１ｍｍ、温度４０℃で行い、摩擦開始直後の静摩擦係数、及び１５分経過時の動摩擦係数を測定し、摩擦停止後、試験球の摩耗痕を測定した。 [Evaluation method]
An evaluation test (measurement of friction coefficient, etc.) of each lubricant composition of Examples 1 to 6 and Comparative Examples 1 to 4 was performed according to the method described below. The results are shown at the bottom of Table 2.
(1) SRV test A ball-on-disk SRV friction tester specified in ASTM D5706 was used. The ball was a ball bearing steel ball of SUJ-2 with a diameter of 10 mm, and the disk was a disk-shaped test piece with a diameter of SUJ-2 of 24 mm and a thickness of 7.85 mm. The surface of the disk was lapped with a roughness (R Z ) of 0.45 to 0.65 μm. The friction test is performed at a load of 50 N, an amplitude of 50 Hz, an amplitude width of 1 mm, and a temperature of 40 ° C., and the static friction coefficient immediately after the start of friction and the dynamic friction coefficient after 15 minutes have been measured. It was measured.

（２）蒸発試験
直径７０ｍｍのガラス製シャーレに各供試サンプルを２ｇ秤量し、液体状のサンプルはそのまま、半固体状のサンプルは均一に薄くのばして、１２０℃の高温槽に静置した。２００時間経過時の質量変化より蒸発減量（質量％）を求めた。 (2) Evaporation test Each test sample was weighed in a glass petri dish having a diameter of 70 mm, the liquid sample was left as it was, the semi-solid sample was uniformly thinned, and left in a high-temperature bath at 120 ° C. The evaporation loss (mass%) was determined from the mass change after 200 hours.

実施例１〜６は、ＳＲＶ摩擦試験において静摩擦係数が０．１３〜０．１７、動摩擦係数が０．１４〜０．１６であり、個々のサンプルの静摩擦係数と動摩擦係数は同じ数値ないしほぼ同じ数値であり、摩耗痕径は０．３１〜０．３６ｍｍと小さく、耐摩耗性に優れている。
一方、基油Ａを用いた比較例１、２の常温で液体のサンプルは、それぞれ静摩擦係数と動摩擦係数がともに０．１６であった。摩耗痕径は０．３８〜０．３７ｍｍと実施例より若干大きいが、耐摩耗性に優れている。しかし、基油Ｃを用いた比較例３と汎用グリースの比較例４は、ともに静摩擦係数０．１０、動摩擦係数０．０７と総じて実施例に比べて低い摩擦係数を示した。試験球の摩耗痕径は、比較例３は０．３６ｍｍと小さかったが、比較例４は０．４５ｍｍと大きい摩耗を示した。
半固体状である実施例１〜６の蒸発減量は、比較例１〜３に比べてはるかに少ないことがわかる。実施例４のグリースは、半固体状であるにもかかわらず、蒸発減量が最も多く、しかも１２０℃、２００時間静置で油と増ちょう剤が分離した。
以上の結果から、本発明の実施例では、極少量の潤滑剤であっても高い動摩擦係数を示し、耐摩耗性も優れ、かつ薄膜状に塗布されても高温下で蒸発しにくく長期にわたって摺動部に摩擦被膜が形成されることがわかる。 In Examples 1 to 6, the SRV friction test has a static friction coefficient of 0.13 to 0.17 and a dynamic friction coefficient of 0.14 to 0.16. The static friction coefficient and the dynamic friction coefficient of each sample are the same numerical value or almost the same. It is a numerical value, the wear scar diameter is as small as 0.31 to 0.36 mm, and it has excellent wear resistance.
On the other hand, both the static friction coefficient and the dynamic friction coefficient of the liquid samples at room temperature of Comparative Examples 1 and 2 using the base oil A were 0.16. The wear scar diameter is 0.38 to 0.37 mm, which is slightly larger than the examples, but is excellent in wear resistance. However, Comparative Example 3 using the base oil C and Comparative Example 4 of the general-purpose grease both showed a coefficient of static friction of 0.10 and a coefficient of dynamic friction of 0.07, which were generally lower than those of the examples. The wear scar diameter of the test ball was as small as 0.36 mm in Comparative Example 3, but Comparative Example 4 showed large wear as 0.45 mm.
It turns out that the evaporation loss of Examples 1-6 which are a semi-solid form is much smaller compared with Comparative Examples 1-3. Although the grease of Example 4 was semi-solid, it had the largest evaporation loss, and the oil and the thickener separated when left at 120 ° C. for 200 hours.
From the above results, in the examples of the present invention, even a very small amount of lubricant exhibits a high coefficient of dynamic friction, excellent wear resistance, and even when applied in a thin film form, it is difficult to evaporate at high temperatures for a long time. It can be seen that a friction coating is formed on the moving part.

以上から明らかなように、本発明による常温で半固体状の潤滑剤組成物は、極少量の使用量で、薄膜状態を形成し、高い動摩擦係数と優れた耐摩耗性を示すとともに蒸発損失されにくく長期にわたって摺動部を潤滑できる。特に高い動摩擦係数は、例えば、ギヤ、ベルト、チェーン、ワイヤーロープ、ヒンジ、機械式無段変速機などの伝動要素機構を有する機械システムに好適に利用することができ、かつ耐摩耗性に優れ、油漏れや蒸発損失が少ないことから機械システムのロングライフ化に貢献することが期待される。   As is clear from the above, the lubricant composition of the present invention at a normal temperature and a semi-solid form forms a thin film state with a very small amount of use, exhibits a high dynamic friction coefficient and excellent wear resistance, and is not evaporated. It is difficult to lubricate the sliding part over a long period of time. A particularly high dynamic friction coefficient can be suitably used for a mechanical system having a transmission element mechanism such as a gear, a belt, a chain, a wire rope, a hinge, and a mechanical continuously variable transmission, and has excellent wear resistance. It is expected to contribute to the long life of mechanical systems due to low oil leakage and evaporation loss.

Claims (3)

％Ｃｐが７０以下であるアルキルナフテン及びアルキルベンゼンから選択される少なくとも１種の炭化水素基油を７０〜９３質量％、５０〜４００ｍｇＫＯＨ／ｇのＣａスルホネート及びＣａサリシレートから選択される少なくとも１種のアルカリ土類金属塩を２〜１０質量％、及び下記一般式（２）で表される少なくとも１種のアミド化合物を５〜２０質量％含み、常温で半固体状であることを特徴とする伝動要素機構に用いる潤滑剤組成物。
〔式（２）において、Ｒ 3 及びＲ 4 は、それぞれ独立して炭素数１２〜２０の飽和又は不飽和の鎖状炭化水素基であり、Ａ 1 は、炭素数１〜１０のアルキレン基である。〕 % Cp is at least one hydrocarbon base oil is selected from alkyl naphthenes and alkyl benzene is 70 or less 70 to 93 wt%, at least one alkali selected from Ca sulfonate and Ca salicylate 50~400mgKOH / g A transmission element characterized in that it contains 2 to 10 % by mass of an earth metal salt and 5 to 20 % by mass of at least one amide compound represented by the following general formula (2) , and is semi-solid at normal temperature Lubricant composition used for mechanism.
[Oite the formula (2), R 3 and R 4 are each independently a chain saturated or unsaturated hydrocarbon group having 12 to 20 carbon atoms, A 1 is alkylene of 1 to 10 carbon atoms It is a group . ] 一般式（２）で表されるアミド化合物は、エチレンビスオレイン酸アミドまたはエチレンビスステアリン酸アミドである請求項１に記載の潤滑剤組成物。 The lubricant composition according to claim 1, wherein the amide compound represented by the general formula (2) is ethylene bisoleic acid amide or ethylene bis stearic acid amide . 伝動要素機構が、ヒンジ又は機械式無段変速機である請求項１又は２に記載の潤滑剤組成物。 The lubricant composition according to claim 1 or 2, wherein the transmission element mechanism is a hinge or a mechanical continuously variable transmission.
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