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JP2008280476A - Lubricant composition and rolling bearing - Google Patents

Lubricant composition and rolling bearing Download PDF

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JP2008280476A
JP2008280476A JP2007127727A JP2007127727A JP2008280476A JP 2008280476 A JP2008280476 A JP 2008280476A JP 2007127727 A JP2007127727 A JP 2007127727A JP 2007127727 A JP2007127727 A JP 2007127727A JP 2008280476 A JP2008280476 A JP 2008280476A
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lubricant composition
acid
urea compound
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rolling bearing
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JP2008280476A5 (en
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Yasunobu Fujita
安伸 藤田
Atsushi Yokouchi
敦 横内
Kaneaki Matsumoto
兼明 松本
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NSK Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a lubricant composition capable of more improving abrasion resistance, durability and reduced torque and to provide a long life rolling bearing having the reduced torque and excellent abrasion resistance and durability. <P>SOLUTION: The lubricant composition is obtained by compounding a base oil with a specific urea compound and a benzylidenesorbitol derivative in the total amount of 10-30 mass%. The rolling bearing comprises the lubricant composition sealed therein. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、各種産業機械や各種モータ、自動車部品等に組み込まれる転がり軸受、並びに前記転がり軸受に好適な潤滑剤組成物に関する。   The present invention relates to a rolling bearing incorporated in various industrial machines, various motors, automobile parts and the like, and a lubricant composition suitable for the rolling bearing.

例えば、各種産業機械や各種モータ、自動車部品に組み込まれる転がり軸受には、潤滑性を付与するためにグリースや潤滑油が使用されている。このうち、グリースは、軸受に密封できるという利点があり、転がり軸受では非常に広く使用されている。反面、潤滑油を供給する油潤滑方式に比べてグリースは流動性が悪いため、転送面への供給性が悪く、潤滑不足から種々の不具合を招く可能性がある。   For example, grease and lubricating oil are used for rolling bearings incorporated in various industrial machines, various motors, and automobile parts in order to impart lubricity. Of these, grease has the advantage that it can be sealed in the bearing, and is widely used in rolling bearings. On the other hand, since grease has poor fluidity compared to an oil lubrication system that supplies lubricating oil, supply to the transfer surface is poor, and various problems may occur due to insufficient lubrication.

このような背景から、増ちょう剤と少量のゲル化剤とを併用することにより、せん断・熱が加えられたときに流動性が発現し、せん断・熱を取り除くと再硬化するグリース組成物が提案されている(特許文献1参照)。   From such a background, by using a thickener and a small amount of gelling agent in combination, a grease composition that exhibits fluidity when shearing / heat is applied and re-cures when shearing / heat is removed is obtained. It has been proposed (see Patent Document 1).

特開昭58−219297号公報JP 58-219297 A

特許文献1に記載のグリース組成物は、転がり軸受の回転時には、軸受転送面では増ちょう剤量が少なくなり発熱が抑えられ、軸受転送面から排出されたグリース組成物はせん断を受けることがないため硬化して漏洩や異物混入を防ぐことができる。しかし、軸受転送面から排出されたグリース組成物が再度軸受転送面に流入しないと、発熱は抑えられても、潤滑不足のために耐摩耗性や耐久性の向上には至らない。   In the grease composition described in Patent Document 1, when the rolling bearing rotates, the amount of the thickener is reduced on the bearing transfer surface and heat generation is suppressed, and the grease composition discharged from the bearing transfer surface is not subjected to shearing. Therefore, it can be hardened to prevent leakage and contamination. However, if the grease composition discharged from the bearing transfer surface does not flow into the bearing transfer surface again, even if heat generation is suppressed, wear resistance and durability are not improved due to insufficient lubrication.

近年、各種産業機械や各種モータ、自動車部品に組み込まれる転がり軸受は、高速化が一層進んでおり、耐摩耗性や耐久性の更なる改善に加え、低トルク化が望まれている。そこで本発明は、適用箇所におけるこれらの特性をより向上させ得る潤滑剤組成物、並びに低トルクで、耐摩耗性や耐久性に優れ長寿命の転がり軸受を提供することを目的とする。   In recent years, rolling bearings incorporated in various industrial machines, various motors, and automobile parts have been further increased in speed, and in addition to further improving wear resistance and durability, lowering of torque is desired. Accordingly, an object of the present invention is to provide a lubricant composition capable of further improving these characteristics at an application site, and a rolling bearing having a low torque, excellent wear resistance and durability, and a long life.

上記課題を解決するために、本発明は下記の潤滑剤組成物及び転がり軸受を提供する。
(1)基油に、下記一般式(1)または(2)で表されるウレア化合物と、ベンジリデンソルビトール誘導体とを合計で10〜30質量%の割合で配合したことを特徴とする潤滑剤組成物。
In order to solve the above problems, the present invention provides the following lubricant composition and rolling bearing.
(1) Lubricant composition characterized in that a urea compound represented by the following general formula (1) or (2) and a benzylidene sorbitol derivative are blended in a base oil in a proportion of 10 to 30% by mass. object.

Figure 2008280476
Figure 2008280476

〔(1)式中、C2m+1及びC2n+1は直鎖アルキル基であり、m+nは16〜36である。また、(2)式中、C2x+1及びC2y+1は直鎖アルキル基であり、x+yは20〜36である。〕
(2)基油がエステル油であることを特徴とする上記(1)記載の潤滑剤組成物。
(3)(ウレア化合物/ベンジリデンソルビトール誘導体)重量比が0.1〜1,0であることを特徴とする上記(1)または(2)記載の潤滑剤組成物。
(4)NSKグリースノイズテスターによるグリースノイズカウントの120秒値が50カウント以下であることを特徴とする上記(1)〜(3)の何れか1項に記載の潤滑剤組成物。
(5)内輪と外輪との間に複数の転動体を転動自在に保持し、かつ、上記(1)〜(4)の何れか1項に記載の潤滑剤組成物を封入したことを特徴とする転がり軸受。
[(1) where, C m H 2m + 1 and C n H 2n + 1 is a straight-chain alkyl group, m + n is 16-36. Further, in (2), C x H 2x + 1 and C y H 2y + 1 is a linear alkyl group, x + y is 20 to 36. ]
(2) The lubricant composition as described in (1) above, wherein the base oil is an ester oil.
(3) The lubricant composition as described in (1) or (2) above, wherein the weight ratio (urea compound / benzylidene sorbitol derivative) is 0.1 to 1.0.
(4) The lubricant composition as described in any one of (1) to (3) above, wherein a grease noise count of 120 seconds by an NSK grease noise tester is 50 counts or less.
(5) A plurality of rolling elements are rotatably held between an inner ring and an outer ring, and the lubricant composition according to any one of (1) to (4) is enclosed. Rolling bearing.

本発明の潤滑剤組成物は、せん断力が加わる状態では油状(降伏値を持たない)となり、せん断力が加わらない状態では固まってゲル状(降伏値の大きい状態)となる。そのため、転がり軸受に封入した場合、転送面から排出されても、保持器とシールとの隙間や転送面付近に存在する潤滑剤組成物スとの接触で生じる極く弱いせん断力により油状となり、転送面に再度供給され、潤滑不足による摩耗が抑えられて長寿命となり、低トルク化も図られる。   The lubricant composition of the present invention becomes oily (having no yield value) in a state where shearing force is applied, and is solidified and gelled (state where the yield value is large) when no shearing force is applied. Therefore, when encapsulated in a rolling bearing, even if it is discharged from the transfer surface, it becomes oily due to the extremely weak shear force generated by contact with the gap between the cage and the seal and the lubricant composition existing near the transfer surface, Re-supplied to the transfer surface, wear due to insufficient lubrication is suppressed, the service life is extended, and the torque is reduced.

以下、本発明に関して詳細に説明する。   Hereinafter, the present invention will be described in detail.

〔潤滑剤組成物〕
本発明の潤滑剤組成物は、基油に、下記一般式(1)または(2)で表されるウレア化合物と、ベンジリデンソルビトール誘導体とを配合したものである。
[Lubricant composition]
The lubricant composition of the present invention is a mixture of a urea compound represented by the following general formula (1) or (2) and a benzylidene sorbitol derivative in a base oil.

Figure 2008280476
Figure 2008280476

(1)式中、C2m+1及びC2n+1は直鎖アルキル基であり、m+nは16〜36である。また、(2)式中、C2x+1及びC2y+1は直鎖アルキル基であり、x+yは20〜36である。 In (1), C m H 2m + 1 and C n H 2n + 1 is a straight-chain alkyl group, m + n is 16-36. Further, in (2), C x H 2x + 1 and C y H 2y + 1 is a linear alkyl group, x + y is 20 to 36.

基油としては、ウレア化合物及びベンジリデンソルビトール誘導体との親和性が高く、これらを完全に溶解できることからエステル油が好ましい。エステル油としては、制限はないが、芳香族系三塩基酸または芳香族系四塩基酸と、分岐アルコールとの反応から得られる芳香族エステル油、一塩基酸と多価アルコールとの反応から得られるポリオールエステル油等を好適に挙げることができる。   As the base oil, ester oil is preferable because it has high affinity with urea compounds and benzylidene sorbitol derivatives and can completely dissolve them. The ester oil is not limited, but is obtained from the reaction of an aromatic tribasic acid or aromatic tetrabasic acid with a branched alcohol and a reaction of a monobasic acid with a polyhydric alcohol. Preferred examples include polyol ester oils.

具体的には、芳香族エステル油としては、芳香族系三塩基酸と分岐アルコールとの反応から得られるエステル油としてピロメリット酸エステル油、トリメシン酸エステル油、具体的にはトリオクチルトリメリテートやトリデシルトリメリテート、芳香族系四塩基酸と分岐アルコールとの反応から得られるピロメリット酸エステル油、具体的にはテトラオクチルピロメリテート等が挙げられる。   Specifically, as the aromatic ester oil, pyromellitic acid ester oil, trimesic acid ester oil, specifically trioctyl trimellitate as ester oil obtained from the reaction of aromatic tribasic acid and branched alcohol. And tridecyl trimellitate, pyromellitic ester oil obtained from a reaction of an aromatic tetrabasic acid and a branched alcohol, specifically tetraoctyl pyromellitate, and the like.

また、ポリオールエステル油としては、以下に示す多価アルコールと一塩基酸とを適宜組み合わせて反応させて得られるものが挙げられる。尚、一塩基酸は単独でもよいし、複数を用いてもよい。更に、多価アルコールと二塩基酸・一塩基酸の混合脂肪酸とのオリゴエステルであるコンプレックスエステルとして用いてもよい。多価アルコールとしては、トリメチロールプロパン、ペンタエリスリトール、ジペンタエリスリトール、ネオペンチルグルコール、2−メチル−2−プロピル−1,3−プロパンジオール等が挙げられる。一方、一塩基酸としては、主に炭素数4〜16の一価脂肪酸が用いられ、具体的には、酪酸、吉草酸、カプロン酸、カプリル酸、エナント酸、ペラルゴン酸、カプリン酸、ウンデカン酸、ラウリン酸、ミステリン酸、パルミチン酸、牛脂脂肪酸、ステアリン酸、カプロレイン酸、パルミトレイン酸、ペトロセリン酸、オレイン酸、エライジン酸、アスクレピン酸、バクセン酸、ソルビン酸、リノール酸、リノイン酸、アビニン酸、リシノール酸等が挙げられる。   Moreover, as a polyol ester oil, what is obtained by making the polyhydric alcohol and monobasic acid shown below react suitably is mentioned. In addition, a monobasic acid may be individual and multiple may be used. Furthermore, you may use as complex ester which is an oligoester of a polyhydric alcohol and the mixed fatty acid of a dibasic acid and a monobasic acid. Examples of the polyhydric alcohol include trimethylolpropane, pentaerythritol, dipentaerythritol, neopentyl glycol, 2-methyl-2-propyl-1,3-propanediol and the like. On the other hand, monobasic acids are mainly monohydric fatty acids having 4 to 16 carbon atoms, specifically, butyric acid, valeric acid, caproic acid, caprylic acid, enanthic acid, pelargonic acid, capric acid, undecanoic acid. , Lauric acid, mysteric acid, palmitic acid, beef tallow fatty acid, stearic acid, caproleic acid, palmitoleic acid, petrothelic acid, oleic acid, elaidic acid, asclepic acid, vaccenic acid, sorbic acid, linoleic acid, linoic acid, abinic acid, ricinol An acid etc. are mentioned.

上記のウレア化合物は、ジイソシアネートと、モノアミンとを反応させて得られる。ジイソシアネートとしては、一般式(1)で表されるウレア化合物ではヘキサメチレンジイソシアネートを、一般式(2)で表されるウレア化合物では4,4´−ジフェニルメタンジイソシアネートを用いる。一方、モノアミンとしては、一般式(1)で表されるウレア化合物では直鎖のC2m+1を有する脂肪族アミン及び直鎖のC2n+1を有する脂肪族アミンを用い、一般式(2)で表されるウレア化合物では直鎖のC2x+1を有する脂肪族アミン及び直鎖のC2y+1を有する脂肪族アミンを用いる。尚、m+nは16〜36であり、x+yは20〜36であるが、炭素数が多いほど基油、特にエステル油との親和性が高く、好ましい。 The urea compound is obtained by reacting diisocyanate with a monoamine. As the diisocyanate, hexamethylene diisocyanate is used in the urea compound represented by the general formula (1), and 4,4′-diphenylmethane diisocyanate is used in the urea compound represented by the general formula (2). On the other hand, as the monoamine, the urea compound represented by the general formula (1) uses an aliphatic amine having linear C m H 2m + 1 and an aliphatic amine having linear C n H 2n + 1. In the urea compound represented by), an aliphatic amine having linear C x H 2x + 1 and an aliphatic amine having linear C y H 2y + 1 are used. In addition, although m + n is 16-36 and x + y is 20-36, the higher the carbon number, the higher the affinity with a base oil, particularly ester oil, which is preferable.

ベンジリデンソルビトール誘導体としては、ジベンジリデンソルビトール、ジトリリデンソルビトール、非対称のジアルキルベンジリデンソルビトール等を好適に挙げることができる。   Preferred examples of the benzylidene sorbitol derivative include dibenzylidene sorbitol, ditrilidene sorbitol, asymmetric dialkyl benzylidene sorbitol, and the like.

ベンジリデンソルビトール誘導体は、数質量%の添加量で基油をNLGI No.2〜No.3程度の硬さに増ちょうできる能力を備えている。また、せん断を受けた時に結晶粒子が分散して流動性を示し、せん断を受けない時には結晶粒子が凝集して流動性を示さなくなるという、流動−復元可逆性を有する。しかし、せん断の有無を繰り返すうちに短時間での構造復元が困難になり、軟化するようになる。そこで、この流動−復元可逆性が緩やかであるウレア化合物を併用することにより、ベンジリデンソルビトール流動体の結晶粒子がウレア化合物の結晶粒子を架橋して再凝集し易くなり、安定した流動−復元可逆性が得られるようになる。   The benzylidene sorbitol derivative is obtained by adding NLGI No. 2-No. It has the ability to increase to about 3 hardness. Further, it has fluidity-reversibility reversibility, in which crystal particles are dispersed to exhibit fluidity when subjected to shearing, and crystal particles aggregate and no longer exhibit fluidity when not subjected to shearing. However, as the presence or absence of shearing is repeated, the structural restoration in a short time becomes difficult and softens. Therefore, by using a urea compound that has a moderate flow-reversibility reversibility, the benzylidene sorbitol fluid crystal particles crosslink the urea compound crystal particles and easily re-aggregate, so that stable fluid-restoration reversibility is achieved. Can be obtained.

このような作用を効果的に得るために、ウレア化合物とベンジリデンソルビトール誘導体とを、(ベンジリデンソルビトール誘導体/ウレア化合物)重量比で0.1〜1.0となるように混合する。この混合比が0.1未満であると、ベンジリデンソルビトール誘導体の結晶粒子の凝集が起こり難く、せん断を受けない時に増ちょう剤網目構造の復元が遅くなり、適用箇所から漏洩しやすくなる。一方、この混合比が1を超えると、分散・凝集の可逆性が損なわれ、漏洩しやすくなる。   In order to effectively obtain such an action, the urea compound and the benzylidene sorbitol derivative are mixed so that the weight ratio of (benzylidene sorbitol derivative / urea compound) is 0.1 to 1.0. When the mixing ratio is less than 0.1, the benzylidene sorbitol derivative crystal particles are less likely to agglomerate, and the restoration of the thickener network structure is delayed when not subjected to shearing, and leakage from the application site is likely. On the other hand, when the mixing ratio exceeds 1, the reversibility of dispersion / aggregation is impaired and leakage tends to occur.

また、ウレア化合物及びベンジリデンソルビトール誘導体は、共に増ちょう剤として機能する。そのため、両者の合計で、潤滑剤組成物全量の10〜30質量%を占めるように配合される。合計での配合量が10質量%未満では潤滑剤組成物が初期から柔らかすぎて適用箇所から漏洩しやすく、30質量%を超える流動性が低く適用箇所に十分な潤滑性を付与できない。   Both urea compounds and benzylidene sorbitol derivatives function as thickeners. Therefore, it mix | blends so that 10-30 mass% of the lubricant composition whole quantity may occupy in total of both. When the total blending amount is less than 10% by mass, the lubricant composition is too soft from the beginning and easily leaks from the application site, the fluidity exceeding 30% by mass is low, and sufficient lubricity cannot be imparted to the application site.

本発明の潤滑剤組成物は、せん断力が加わる状態ではウレア化合物とベンジリデンソルビトール誘導体とからなる網目構造が切断され、ウレア化合物の結晶粒子及びベンジリデンソルビトール誘導体の結晶粒子が配向され著しい硬さ変化が起こり、油状となる。一方、せん断が加わらない状態では網目構造が復元してゲル状となる。従って、転がり軸受に封入した場合、作動時に一部の潤滑剤組成物は転送面から排出されても、保持器とシールとの隙間や転送面付近に存在する潤滑剤組成物と接触すると、極く弱いせん断力が加わり流動性が付与され、転送面に再度供給される。このように、潤滑剤組成物は、潤滑油に近い良好な流動性を有し、低トルクで、耐久性能が良好となる。また、シールに付着した潤滑剤組成物は、せん断力が加わらない状態となるため、ゲル状となり漏洩を防止することもできる。   In the lubricant composition of the present invention, in a state where shearing force is applied, the network structure composed of the urea compound and the benzylidene sorbitol derivative is cut, and the crystal particles of the urea compound and the crystal particles of the benzylidene sorbitol derivative are oriented to cause a significant change in hardness. Occurs and becomes oily. On the other hand, in a state where no shear is applied, the network structure is restored to become a gel. Therefore, when encapsulated in a rolling bearing, even if a part of the lubricant composition is discharged from the transfer surface during operation, if it comes into contact with the lubricant composition existing in the gap between the cage and the seal or in the vicinity of the transfer surface, A weak shear force is applied to impart fluidity, and it is supplied again to the transfer surface. Thus, the lubricant composition has good fluidity close to that of lubricating oil, has low torque, and has good durability performance. Further, since the lubricant composition attached to the seal is in a state where no shearing force is applied, it can be gelled to prevent leakage.

潤滑剤組成物には、その用途に応じて添加剤を配合することにより、各種性能を向上させることができる。例えば、揺動運動用転がり軸受の潤滑に使用する場合、アミン系、フェノール系、硫黄系、ジチオリン酸亜鉛、ジチオカルバミン酸亜鉛等の酸化防止剤;スルホン酸金属塩、エステル系、アミン系、ナフテン酸金属塩、コハク酸誘導体等の防錆剤;リン系、ジチオリン酸亜鉛、有機モリブデン等の極圧剤;脂肪酸、動植物油等の油性向上剤;ベンゾトリアゾール等の金属不活性化剤等をそれぞれ単独で、あるいは適宜組み合わせて添加することができる。尚、これら添加剤の添加量は、本発明の目的を損なわない範囲であれば特に制限されるものではない。   Various performances can be improved by adding an additive to the lubricant composition depending on the application. For example, when used to lubricate rolling bearings for rocking motion, antioxidants such as amines, phenols, sulfurs, zinc dithiophosphates and zinc dithiocarbamates; metal sulfonates, esters, amines, naphthenic acids Rust preventives such as metal salts and succinic acid derivatives; extreme pressure agents such as phosphorus, zinc dithiophosphate and organic molybdenum; oiliness improvers such as fatty acids and animal and vegetable oils; metal deactivators such as benzotriazole Or can be added in appropriate combination. In addition, the addition amount of these additives will not be restrict | limited especially if it is a range which does not impair the objective of this invention.

[転がり軸受]
本発明はまた、上記の潤滑剤組成物を封入した転がり軸受を提供する。転がり軸受の種類や構造には制限がなく、例えば図1に断面図で示す玉軸受1を例示するが、内輪10と外輪11との間に、保持器12を介して複数の転動体である玉13を転動自在に保持し、内輪10と外輪11との間に上記の潤滑剤組成物Gを充填し、シール部材14で封止して構成される。
[Rolling bearings]
The present invention also provides a rolling bearing encapsulating the above-described lubricant composition. There is no limitation on the type and structure of the rolling bearing. For example, the ball bearing 1 shown in a cross-sectional view in FIG. 1 is illustrated, but a plurality of rolling elements are provided between the inner ring 10 and the outer ring 11 via a cage 12. The ball 13 is rotatably held, filled with the lubricant composition G between the inner ring 10 and the outer ring 11, and sealed with a seal member 14.

本発明の転がり軸受は、上記したように、潤滑剤組成物の作用により、送面に再供給され、潤滑不足による摩耗が抑えられて長寿命となり、低トルク化も図られている。   As described above, the rolling bearing of the present invention is re-supplied to the feeding surface by the action of the lubricant composition, wear due to insufficient lubrication is suppressed, the life is extended, and the torque is reduced.

以下に実施例及び比較例を挙げて本発明を更に説明するが、本発明はこれにより何ら制限されるものではない。   Examples The present invention will be further described below with reference to examples and comparative examples, but the present invention is not limited thereby.

(実施例1)
第1の容器にて、42部のペンタエリスリトールエステル(PET)にヘキサメチレンジイソシアネート(HDI)を4部添加して溶解し、70℃まで加熱した。第2の容器にて、45部のPETにオクチルアミン(CNH)を6部溶解した。そして、第1の容器に第2の容器の内容物を入れ、攪拌しながら徐々に昇温して140℃で30分保持してウレア化合物を合成した。次いで、第1の容器にジベンジリデンソルビトール(DBS)を3部添加し、十分に攪拌して混合した後、195℃まで昇温してウレア化合物とDBSとを完全に溶解させた。次いで、予め水冷したアルミニウム製バットに第1の容器の内容物を流し込み、バットを流水で冷却することでゲル状物を得た。そして、ゲル状物を3本ロールミルにかけて供試潤滑剤組成物を得た。
Example 1
In a first container, 4 parts of hexamethylene diisocyanate (HDI) was added and dissolved in 42 parts of pentaerythritol ester (PET) and heated to 70 ° C. In a second container, 6 parts of octylamine (C 8 NH 2 ) was dissolved in 45 parts of PET. And the content of the 2nd container was put into the 1st container, and it heated up gradually, stirring, and hold | maintained at 140 degreeC for 30 minutes, and synthesize | combined the urea compound. Next, 3 parts of dibenzylidene sorbitol (DBS) was added to the first container, and after sufficiently stirring and mixing, the temperature was raised to 195 ° C. to completely dissolve the urea compound and DBS. Next, the contents of the first container were poured into an aluminum bat that had been previously water-cooled, and the bat was cooled with running water to obtain a gel-like material. Then, a gel lubricant was put on a three-roll mill to obtain a test lubricant composition.

(実施例2〜6)
表1に示す基油、ジイソシアネート、モノアミン及びベンジリデンソルビトール誘導体を用い、実施例1に準じて供試潤滑剤組成物を得た。
(Examples 2 to 6)
A test lubricant composition was obtained according to Example 1 using the base oil, diisocyanate, monoamine and benzylidene sorbitol derivative shown in Table 1.

(比較例1)
PET中で、4,4´−ジフェニルメタンジイソシアネート(MDI)とシクロへキシルアミン(CHA)とを反応させてウレア化合物を合成し、供試潤滑剤組成物を得た。
(Comparative Example 1)
In PET, 4,4′-diphenylmethane diisocyanate (MDI) and cyclohexylamine (CHA) were reacted to synthesize a urea compound to obtain a test lubricant composition.

(比較例2)
PETにDBSを添加して供試潤滑剤組成物を得た。
(Comparative Example 2)
DBS was added to PET to obtain a test lubricant composition.

(比較例3)
鉱油(MO)に、12ヒドロキシステアリン酸リチウム及びDBSを配合して供試潤滑剤組成物を得た。
(Comparative Example 3)
A test lubricant composition was obtained by blending 12 hydroxylithium stearate and DBS with mineral oil (MO).

(比較例4)
MO中で、MDIとp−トルイジンとを反応させてウレア化合物を合成し、N−アシルアミノ酸ジアミドを添加して供試潤滑剤組成物を得た。
(Comparative Example 4)
In MO, MDI and p-toluidine were reacted to synthesize a urea compound, and N-acylamino acid diamide was added to obtain a test lubricant composition.

(比較例5)
PET中で、HDIとCNHとを反応させてウレア化合物を合成し、供試潤滑剤組成物を得た。
(Comparative Example 5)
In PET, HDI and C 8 NH 2 were reacted to synthesize a urea compound to obtain a test lubricant composition.

(比較例6)
PET中で、トリレンジイソシアネート(TDI)とCNHとを反応させてウレア化合物を合成し、DBSを添加して供試潤滑剤組成物を得た。
(Comparative Example 6)
Toluene diisocyanate (TDI) and C 8 NH 2 were reacted in PET to synthesize a urea compound, and DBS was added to obtain a test lubricant composition.

上記の各供試潤滑剤組成物について、下記の評価を行なった。   The following evaluation was performed for each of the above-described lubricant compositions.

(1)せん断の有無と見かけ粘度との関係
実施例1の供試潤滑剤組成物と比較例1の供試潤滑剤組成物とを用い、初期の見かけ粘度(図中●)、せん断を1回受けた後の見かけ粘度(図中▲)、せん断を1回受け所定時間放置した後の見かけ粘度(図中■)、放置後更にせん断を受けたとき(せん断2回目)の見かけ粘度(図中◆)を測定した。図2に実施例1の供試潤滑剤組成物の測定結果を示すが、せん断を受けたときに油状となって流動性を示し、放置すると元の硬さのゲル状に戻る特性を有することがわかる。一方、図3に比較例1の供試潤滑剤組成物の測定結果を示すが、ウレア化合物のみを含むため、せん断を受けた時と放置時とで見かけ粘度の変化が少ない。
(1) Relationship between presence / absence of shear and apparent viscosity Using the test lubricant composition of Example 1 and the test lubricant composition of Comparative Example 1, the initial apparent viscosity (● in the figure) and shear were 1 Apparent viscosity after receiving (▲ in the figure), apparent viscosity after receiving a shear for a specified time (■ in the figure), and apparent viscosity after further shearing (second shear) (Figure) Medium ◆) was measured. FIG. 2 shows the measurement results of the test lubricant composition of Example 1, which is oily and fluid when subjected to shearing, and has the property of returning to a gel with the original hardness when left untreated. I understand. On the other hand, FIG. 3 shows the measurement result of the test lubricant composition of Comparative Example 1. Since only the urea compound is contained, the change in the apparent viscosity is small when subjected to shearing and when left standing.

(2)混和ちょう度、不混和ちょう度の評価
各供試潤滑剤組成物について、混和ちょう度(60W)と不混和ちょう度(0W)との差を求めた。結果を表1及び表2に示すが、50以上を合格とした。
(2) Evaluation of blending penetration and immiscibility penetration For each sample lubricant composition, the difference between the blending penetration (60 W) and the immiscibility penetration (0 W) was determined. Although a result is shown in Table 1 and Table 2, 50 or more was set as the pass.

(3)流動−復元可逆性試験
各供試潤滑剤組成物を、自転−公転式攪拌機(せん断条件:自転1370r/min、公転1370r/min、3min)で攪拌して不混和ちょう度を測定した後、40℃で3時間放置して不混和ちょう度を測定するサイクルを4回繰り返した。結果を表1及び表2に示すが、1回目のせん断後の不混和ちょう度と、2〜4回のせん断後の各不混和ちょう度との差、並びに1回目の放置後の不混和ちょう度と、2〜4回目の放置後の各不混和ちょう度との差が、何れも±15以内であれば、良好な流動−復元可逆性を有すると見なすことができ、各実施例の供試潤滑剤組成物はこの基準を満足している。
(3) Flow-recovery reversibility test Each lubricant composition was stirred with a rotation-revolution stirrer (shear conditions: rotation 1370 r / min, revolution 1370 r / min, 3 min), and the immiscible consistency was measured. Thereafter, the cycle of leaving the mixture at 40 ° C. for 3 hours and measuring the immiscible penetration was repeated 4 times. The results are shown in Tables 1 and 2, and the difference between the immiscible penetration after the first shearing and the respective immiscibility penetrations after the 2nd to 4th shearing, and the immiscibility after the first standing. And the immiscible penetration after 2nd to 4th exposure are all within ± 15, it can be regarded as having good flow-restoration reversibility. The test lubricant composition satisfies this criterion.

また、図4に、実施例1、比較例1及び比較例2の各供試潤滑剤組成物の測定結果をグラフ化して示すが、比較例1及び比較例2の供試潤滑剤組成物は、攪拌と放置とを繰り返すうちに、放置後の不混和ちょう度の上昇が大きく、流動−復元可逆性が低下している。   FIG. 4 is a graph showing the measurement results of the test lubricant compositions of Example 1, Comparative Example 1 and Comparative Example 2. The test lubricant compositions of Comparative Example 1 and Comparative Example 2 are shown in FIG. As the stirring and leaving are repeated, the increase in the immiscibility after standing is large and the flow-restoration reversibility is lowered.

(4)軸受トルク試験
非接触シール付きの単列深溝玉軸受(内径25mm、外径62mm、幅17mm)に各供試潤滑剤組成物を充填して供試軸受を作製した。そして、供試軸受を、回転数3000r/min、アキシアル荷重98N,ラジアル荷重98Nにて180秒間回転させた後、回転トルクを測定した。結果を表1及び表2に示すが、比較例1に対する相対値で示してある。このトルク相対値1.0未満を合格としたが、実施例の供試軸受は何れも前記基準を満たしている。
(4) Bearing torque test Single-row deep groove ball bearings with a non-contact seal (inner diameter 25 mm, outer diameter 62 mm, width 17 mm) were filled with each test lubricant composition to prepare test bearings. The test bearing was rotated for 180 seconds at a rotational speed of 3000 r / min, an axial load of 98 N, and a radial load of 98 N, and then the rotational torque was measured. The results are shown in Tables 1 and 2, but are shown as relative values with respect to Comparative Example 1. Although this torque relative value of less than 1.0 was determined to be acceptable, all of the test bearings of the examples satisfied the above criteria.

(5)軸受漏洩試験
非接触シール付きの単列深溝玉軸受(内径25mm、外径62mm、幅17mm)に各供試潤滑剤組成物を充填して供試軸受を作製した。そして、供試軸受を、回転数10000r/min、アキシアル荷重98N,ラジアル荷重98Nにて20時間連続回転させ、初期重量との差からグリース漏洩率を求めた。結果を表1に示すが、グリース漏洩率6質量%以下を合格とした。実施例の供試軸受は、何れも前記基準を満たしている。
(5) Bearing leakage test Single-row deep groove ball bearings with a non-contact seal (inner diameter 25 mm, outer diameter 62 mm, width 17 mm) were filled with each test lubricant composition to prepare test bearings. The test bearing was continuously rotated for 20 hours at a rotational speed of 10000 r / min, an axial load of 98 N, and a radial load of 98 N, and the grease leakage rate was determined from the difference from the initial weight. The results are shown in Table 1. A grease leakage rate of 6% by mass or less was accepted. The test bearings of the examples all satisfy the above criteria.

また、実施例1に従い、(ベンジリデンソルビトール誘導体/ウレア化合物)重量比を変えて供試潤滑剤組成物を調製し、同様にしてグリース漏洩率を求めた。結果を図5に示すが、(ベンジリデンソルビトール誘導体/ウレア化合物)重量比が1の供試軸受に対する相対値で示してある。同図から、(ベンジリデンソルビトール誘導体/ウレア化合物)重量比が0.1〜1.0の範囲であればグリース漏洩を極力抑え得ることがわかる。   In addition, according to Example 1, test lubricant compositions were prepared by changing the weight ratio of (benzylidene sorbitol derivative / urea compound), and the grease leakage rate was determined in the same manner. The results are shown in FIG. 5 and are shown as relative values with respect to the test bearing having a (benzylidene sorbitol derivative / urea compound) weight ratio of 1. From the figure, it can be seen that when the weight ratio of (benzylidene sorbitol derivative / urea compound) is in the range of 0.1 to 1.0, grease leakage can be suppressed as much as possible.

(6)グリースノイズ試験
非接触シール付きの単列深溝玉軸受(内径15mm、外径35mm、幅11mm)に各供試潤滑剤組成物を充填して供試軸受を作製した。そして、供試軸受を、回転数1800r/min、アキシアル荷重29.4Nにて120秒間回転させた後、NSKグリースノイズテスターを用い、軸受ラジアル方向の振動による規定値以上のパスル値を計測した。結果を表1及び表2に示すが、このグリースノイズカウントの120秒値が50カウント以下を合格とした。実施例の供試軸受は、何れも前記基準を満たしている。
(6) Grease noise test A single-row deep groove ball bearing with a non-contact seal (inner diameter 15 mm, outer diameter 35 mm, width 11 mm) was filled with each test lubricant composition to prepare a test bearing. Then, after rotating the test bearing for 120 seconds at a rotational speed of 1800 r / min and an axial load of 29.4 N, a pulse value greater than a prescribed value due to vibration in the bearing radial direction was measured using an NSK grease noise tester. The results are shown in Table 1 and Table 2, and the grease noise count of 120 seconds was determined to be 50 counts or less. The test bearings of the examples all satisfy the above criteria.

Figure 2008280476
Figure 2008280476

Figure 2008280476
Figure 2008280476

本発明の転がり軸受の一例である玉軸受を示す断面図である。It is sectional drawing which shows the ball bearing which is an example of the rolling bearing of this invention. 実施例1の供試潤滑剤組成物におけるせん断応力と見かけ粘度との関係を示すグラフである。2 is a graph showing the relationship between shear stress and apparent viscosity in the test lubricant composition of Example 1. FIG. 比較例1の供試潤滑剤組成物におけるせん断応力と見かけ粘度との関係を示すグラフである。6 is a graph showing the relationship between shear stress and apparent viscosity in the test lubricant composition of Comparative Example 1. 実施例における(3)流動−復元可逆性試験の結果を示すグラフである。It is a graph which shows the result of the (3) flow-restoration reversibility test in an Example. 実施例で得られた(ベンジリデンソルビトール誘導体/ウレア化合物)重量比とグリース漏洩率との関係を示すグラフである。It is a graph which shows the relationship between the weight ratio obtained in the Example (benzylidene sorbitol derivative / urea compound) and the grease leakage rate.

符号の説明Explanation of symbols

1 玉軸受
10 内輪
11 外輪
12 保持器
13 玉
14 シール部材
G 潤滑剤組成物
DESCRIPTION OF SYMBOLS 1 Ball bearing 10 Inner ring 11 Outer ring 12 Cage 13 Ball 14 Seal member
G Lubricant composition

Claims (5)

基油に、下記一般式(1)または(2)で表されるウレア化合物と、ベンジリデンソルビトール誘導体とを合計で10〜30質量%の割合で配合したことを特徴とする潤滑剤組成物。
Figure 2008280476
〔(1)式中、C2m+1及びC2n+1は直鎖アルキル基であり、m+nは16〜36である。また、(2)式中、C2x+1及びC2y+1は直鎖アルキル基であり、x+yは20〜36である。〕
A lubricant composition comprising a base oil and a urea compound represented by the following general formula (1) or (2) and a benzylidene sorbitol derivative in a proportion of 10 to 30% by mass in total.
Figure 2008280476
[(1) where, C m H 2m + 1 and C n H 2n + 1 is a straight-chain alkyl group, m + n is 16-36. Further, in (2), C x H 2x + 1 and C y H 2y + 1 is a linear alkyl group, x + y is 20 to 36. ]
基油がエステル油であることを特徴とする請求項1記載の潤滑剤組成物。   The lubricant composition according to claim 1, wherein the base oil is an ester oil. (ウレア化合物/ベンジリデンソルビトール誘導体)重量比が0.1〜1,0であることを特徴とする請求項1または2記載の潤滑剤組成物。   The lubricant composition according to claim 1 or 2, wherein a weight ratio of (urea compound / benzylidene sorbitol derivative) is 0.1 to 1,0. NSKグリースノイズテスターによるグリースノイズカウントの120秒値が50カウント以下であることを特徴とする請求項1〜3の何れか1項に記載の潤滑剤組成物。   The lubricant composition according to any one of claims 1 to 3, wherein a grease noise count of 120 seconds by an NSK grease noise tester is 50 counts or less. 内輪と外輪との間に複数の転動体を転動自在に保持し、かつ、請求項1〜4の何れか1項に記載の潤滑剤組成物を封入したことを特徴とする転がり軸受。   A rolling bearing characterized in that a plurality of rolling elements are rotatably held between an inner ring and an outer ring, and the lubricant composition according to any one of claims 1 to 4 is enclosed.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010126635A (en) * 2008-11-27 2010-06-10 Nsk Ltd Lubricant composition and rolling device
JP2010156392A (en) * 2008-12-26 2010-07-15 Nsk Ltd Rolling bearing
JP2010196727A (en) * 2009-02-23 2010-09-09 Nsk Ltd Rolling bearing
JP2010209129A (en) * 2009-03-06 2010-09-24 Nsk Ltd Grease composition and rolling bearing
JP2013234294A (en) * 2012-05-10 2013-11-21 Nsk Ltd Lubricant composition and rolling bearing
JP2014074101A (en) * 2012-10-03 2014-04-24 Nsk Ltd Rolling device
JP7480399B2 (en) 2022-08-01 2024-05-09 セイコーインスツル株式会社 Grease

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JPS4916705A (en) * 1972-06-03 1974-02-14
JPS5531847A (en) * 1978-08-29 1980-03-06 Honda Motor Co Ltd Gelled grease
JPS58219297A (en) * 1982-06-16 1983-12-20 Kyodo Yushi Kk Grease composition
JPS5911398A (en) * 1982-07-10 1984-01-20 Kyodo Yushi Kk Lubrication

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JPS4916705A (en) * 1972-06-03 1974-02-14
JPS5531847A (en) * 1978-08-29 1980-03-06 Honda Motor Co Ltd Gelled grease
JPS58219297A (en) * 1982-06-16 1983-12-20 Kyodo Yushi Kk Grease composition
JPS5911398A (en) * 1982-07-10 1984-01-20 Kyodo Yushi Kk Lubrication

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010126635A (en) * 2008-11-27 2010-06-10 Nsk Ltd Lubricant composition and rolling device
JP2010156392A (en) * 2008-12-26 2010-07-15 Nsk Ltd Rolling bearing
JP2010196727A (en) * 2009-02-23 2010-09-09 Nsk Ltd Rolling bearing
JP2010209129A (en) * 2009-03-06 2010-09-24 Nsk Ltd Grease composition and rolling bearing
JP2013234294A (en) * 2012-05-10 2013-11-21 Nsk Ltd Lubricant composition and rolling bearing
JP2014074101A (en) * 2012-10-03 2014-04-24 Nsk Ltd Rolling device
JP7480399B2 (en) 2022-08-01 2024-05-09 セイコーインスツル株式会社 Grease

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