JP2009007425A - Non-diffusibile fluorine grease composition - Google Patents
Non-diffusibile fluorine grease composition Download PDFInfo
- Publication number
- JP2009007425A JP2009007425A JP2007168468A JP2007168468A JP2009007425A JP 2009007425 A JP2009007425 A JP 2009007425A JP 2007168468 A JP2007168468 A JP 2007168468A JP 2007168468 A JP2007168468 A JP 2007168468A JP 2009007425 A JP2009007425 A JP 2009007425A
- Authority
- JP
- Japan
- Prior art keywords
- oil
- fluorine
- grease
- diffusion
- silicone oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Lubricants (AREA)
Abstract
Description
本発明は、グリース中の油分が部材表面で拡散しない非拡散性のフッ素グリース組成物に関する。 The present invention relates to a non-diffusible fluorine grease composition in which oil in a grease does not diffuse on the surface of a member.
各種機構部品において潤滑剤は不可欠であり、各種の部位で多くの潤滑油剤が使用されている。例えばグリース製品は、潤滑油剤を機構部品に保持して流出を防止する目的で、油成分を増稠剤と呼ばれる物質で半固体状としたものである。 Lubricants are indispensable in various mechanical parts, and many lubricants are used in various parts. For example, a grease product is a semi-solid oil component made of a material called a thickener for the purpose of holding a lubricating oil in a mechanical part to prevent outflow.
しかしながら、このグリース製品でも油の滲み出し防止は完全ではなく、各種の基油拡散防止剤が提案されている。例えば、特開平8−176575号公報には、合成潤滑油を基油とするグリースへの拡散防止剤として、パーフルオロカーボンチェーンを持ち、且つ親水基としてポリオキシエチレンを持つフッ素系の界面活性剤が記載されている。しかしながら、このフッ素系界面活性剤は、基油の拡散防止性能が充分とはいえなかった。 However, even this grease product does not completely prevent oil oozing, and various base oil diffusion inhibitors have been proposed. For example, JP-A-8-176575 discloses a fluorosurfactant having a perfluorocarbon chain and having a polyoxyethylene as a hydrophilic group as an anti-diffusion agent for grease based on synthetic lubricating oil. Are listed. However, this fluorosurfactant was not sufficient in the base oil diffusion preventing performance.
また、特開2000−109874号公報には、フッ素系グリースにシリコーンオイルを0.1〜50%混合した非拡散性のフッ素グリース組成物が開示されている。しかしながら、低粘度のフッ素オイルでは、充分な拡散防止性能が得られない。また、シリコーンオイルを含むことで、特に金属対金属間での耐荷重能が低下してしまい、その配合量によってはフッ素オイルのもつ耐荷重能を低下させるという問題があった。 Japanese Patent Application Laid-Open No. 2000-109874 discloses a non-diffusible fluorine grease composition in which 0.1 to 50% of silicone oil is mixed with fluorine grease. However, sufficient anti-diffusion performance cannot be obtained with low-viscosity fluorine oil. In addition, the inclusion of silicone oil reduces the load bearing capacity, particularly between metal and metal, and there is a problem that the load bearing capacity of the fluorine oil is lowered depending on the amount of the blend.
本発明は、上記した従来の事情に鑑みてなされたものであり、基油であるフッ素オイルの拡散が極めて少ないフッ素グリース組成物を提供することを目的とするものである。 The present invention has been made in view of the above-described conventional circumstances, and an object thereof is to provide a fluorine grease composition in which the diffusion of fluorine oil as a base oil is extremely small.
本発明者は、フッ素グリースの主要成分であるフッ素オイルの拡散機構について検討した結果、以下の知見を得た。フッ素オイルの拡散は、フッ素グリースを塗布した部材表面にフッ素オイル分子が吸着することから始まる。従って、フッ素オイルの拡散を防止するには、フッ素と反発しあう異種物質を、フッ素オイル分子より速く吸着させることが有効であると考えた。 As a result of examining the diffusion mechanism of fluorine oil, which is the main component of fluorine grease, the present inventor has obtained the following knowledge. The diffusion of fluorine oil starts from the adsorption of fluorine oil molecules on the surface of the member to which fluorine grease is applied. Therefore, in order to prevent the diffusion of fluorine oil, it was considered effective to adsorb different substances repelling with fluorine faster than fluorine oil molecules.
その結果、フッ素オイルの拡散防止に有効な物質として、フッ素オイル分子より運動速度が高い、即ち、より低分子量であり、運動速度を代用する物性として動粘度がフッ素オイルと同等又はそれ以下であり、且つ、分子としての吸着力がフッ素オイルより強固な、評価基準として接触角の数値がフッ素オイル以下である物質が望ましいことが分った。 As a result, as a substance effective in preventing the diffusion of fluorine oil, the kinetic speed is higher than that of the fluorinated oil molecule, that is, the molecular weight is lower, and the kinematic viscosity is equivalent to or less than that of the fluorinated oil as a physical property that substitutes the kinetic speed. In addition, it has been found that a substance having an adsorption force as a molecule stronger than that of fluorine oil and a numerical value of contact angle of fluorine oil or less as an evaluation criterion is desirable.
そこで、本発明においては、本質的に上記機能を持つシリコーンオイルを基油拡散防止のための主成分とすると共に、窒素を含有する界面活性剤を併用することで、塗布した部材表面でシリコーンオイルの表面張力を著しく低減できることを見出し、両者の相乗効果によりシリコーンオイル単独では到達できなかったフッ素オイルの拡散防止能を驚異的に低減することができた。 Therefore, in the present invention, the silicone oil essentially having the above functions is used as a main component for preventing base oil diffusion, and a surfactant containing nitrogen is used in combination so that the silicone oil is applied to the surface of the applied member. It was found that the surface tension of the fluorine oil can be remarkably reduced, and the synergistic effect of the two has dramatically reduced the ability to prevent the diffusion of fluorine oil, which could not be achieved with silicone oil alone.
即ち、上記目的を達成するため、本発明が提供する非拡散性フッ素グリース組成物は、基油であるフッ素オイルと増稠剤を含むフッ素グリースに、シリコーンオイル0.1〜10重量%と含窒素系界面活性剤0.1〜5.0重量%を添加したことを特徴とするものである。また、前記シリコーンオイルとしては、40℃の動粘度が1〜500mm2/sであることが好ましい。 That is, in order to achieve the above object, the non-diffusible fluorine grease composition provided by the present invention contains 0.1 to 10% by weight of silicone oil in a fluorine grease containing a base oil and a thickener. This is characterized in that 0.1 to 5.0% by weight of a nitrogen-based surfactant is added. The silicone oil preferably has a kinematic viscosity at 40 ° C. of 1 to 500 mm 2 / s.
本発明によれば、フッ素グリースから基油のフッ素オイルが離油することを防ぎ、フッ素オイルの拡散を従来よりも著しく小さくすることができる。従って、潤滑に供する部分にのみフッ素オイルが存在し、その他の部分にはフッ素オイルが流失しない、非拡散性に優れたグリース組成物を提供することができる。 According to the present invention, it is possible to prevent the fluorine oil of the base oil from separating from the fluorine grease, and to significantly reduce the diffusion of the fluorine oil as compared with the prior art. Therefore, it is possible to provide a grease composition excellent in non-diffusibility, in which fluorine oil is present only in the portion to be lubricated and fluorine oil is not washed away in the other portions.
本発明による非拡散性フッ素グリース組成物は、フッ素オイルに増稠剤を添加してグリース化した通常のフッ素系グリースに、シリコーンオイルと含窒素系界面活性剤を添加混合したものである。フッ素オイルには、大別して直鎖タイプと側鎖タイプがあり、40℃での動粘度が1000mm2/s前後の高粘度品から、40℃での動粘度が15mm2/s程度の低粘度品まで様々の種類がある。また、増稠剤としては、ポリテトラフルオロエチレン(PTFE)などが一般に使用されている。 The non-diffusible fluorine grease composition according to the present invention is obtained by adding silicone oil and a nitrogen-containing surfactant to a normal fluorine-based grease that is made into a grease by adding a thickener to fluorine oil. The fluorine oil has roughly classified into linear type and side chain type, low viscosity kinematic viscosity from high viscosity products 1000 mm 2 / s before and after, the kinematic viscosity at 40 ° C. of about 15 mm 2 / s at 40 ° C. There are various types of goods. Moreover, polytetrafluoroethylene (PTFE) etc. are generally used as a thickener.
本発明で用いるシリコーンオイルとしては、ジメチルシリコーンオイルをはじめ、フェニル変性、カルボキシル変性、アミン変性など、従来から知られている各種のシリコーンオイルを使用することができる。これらシリコーンオイルの中でも、動粘度が40℃で1〜500mm2/sのものが好ましい、40℃での動粘度が1mm2/s未満では拡散防止効果が小さいうえ、高温又は低真空下で蒸発しやすい。また、40℃での動粘度が500mm2/sを超えた場合にも、拡散防止効果が小さくなるため好ましくない。 As the silicone oil used in the present invention, various conventionally known silicone oils such as dimethyl silicone oil, phenyl-modified, carboxyl-modified and amine-modified can be used. Among these silicone oils, kinematic viscosity preferably from 1 to 500 mm 2 / s at 40 ° C., after a kinematic viscosity at 40 ° C. is less diffusion preventing effect is less than 1 mm 2 / s, evaporation under a high-temperature or low vacuum It's easy to do. Also, when the kinematic viscosity at 40 ° C. exceeds 500 mm 2 / s, the effect of preventing diffusion is reduced, which is not preferable.
また、上記シリコーンオイルの配合量は、フッ素グリース組成物全体の0.1〜10重量%の範囲とする。シリコーンオイルの配合量が0.1重量%未満では、拡散防止効果が得られない。逆にシリコーンオイルの配合量が10重量%を超えると、シリコーンオイルの影響が大きくなり、耐荷重能をはじめフッ素オイルの持つ性能が低減する。また、シリコーンオイルが10重量%を超えると、増稠剤であるポリテトラフルオロエチレンとの相性が悪いために、グリースから油分離が起こる可能性がある。 The blending amount of the silicone oil is in the range of 0.1 to 10% by weight of the whole fluorine grease composition. When the blending amount of the silicone oil is less than 0.1% by weight, the diffusion preventing effect cannot be obtained. On the other hand, when the blending amount of the silicone oil exceeds 10% by weight, the influence of the silicone oil becomes large, and the performance of the fluorine oil including the load bearing capacity decreases. On the other hand, if the silicone oil exceeds 10% by weight, the oil may be separated from the grease due to poor compatibility with polytetrafluoroethylene as a thickener.
本発明で用いる含窒素系界面活性剤としては、アミド系の脂肪酸アルカノールアミド、脂肪酸モノエタノールアミド、脂肪酸トリエタノールアミド、ポリオキシエチレン脂肪酸アミドなどと、アミン系のポリオキシエチレンアルキルアミン、アルキルアミンエチレンオキシド付加体などを好適に使用することができる。特にアミン系の含窒素系界面活性剤は、シリコーンオイルとの拡散防止性能の向上に対する相乗効果が大きく好ましい。 Examples of nitrogen-containing surfactants used in the present invention include amide fatty acid alkanolamides, fatty acid monoethanolamides, fatty acid triethanolamides, polyoxyethylene fatty acid amides, amine-based polyoxyethylene alkylamines, and alkylamine ethylene oxides. An adduct or the like can be preferably used. In particular, amine-based nitrogen-containing surfactants are preferable because they have a great synergistic effect on the improvement of diffusion preventing performance with silicone oil.
上記含窒素系界面活性剤の配合量は、フッ素グリース組成物全体の0.1〜5.0重量%の範囲とする。含窒素系界面活性剤の配合量が0.1重量%よりも少ない場合、シリコーンオイルとの拡散防止性能の向上に対する相乗効果はほとんど認められなくなる。また、含窒素系界面活性剤の配合量を5.0重量%より増やしても、拡散防止性能に与える添加効果は頭打ちとなる。 The blending amount of the nitrogen-containing surfactant is in the range of 0.1 to 5.0% by weight of the whole fluorine grease composition. When the blending amount of the nitrogen-containing surfactant is less than 0.1% by weight, a synergistic effect for improving the diffusion preventing performance with the silicone oil is hardly recognized. Moreover, even if the blending amount of the nitrogen-containing surfactant is increased from 5.0% by weight, the effect of adding to the diffusion preventing performance reaches a peak.
フッ素オイル、増稠剤、シリコーンオイル、界面活性剤を混合して、下記表1に示す試料1〜9の組成を有するフッ素グリース組成物を作製した。基油であるフッ素オイルは、ダイキン工業株式会社製のデムナムS−20(動粘度は40℃で約20mm2/s)を使用した。増稠剤としては、三井・デュポンフルオロケミカル株式会社製のPTFEを使用した。 Fluorine grease, thickener, silicone oil, and surfactant were mixed to prepare fluorine grease compositions having the compositions of Samples 1 to 9 shown in Table 1 below. As the fluorine oil as the base oil, demnum S-20 (dynamic viscosity is about 20 mm 2 / s at 40 ° C.) manufactured by Daikin Industries, Ltd. was used. As the thickener, PTFE manufactured by Mitsui DuPont Fluorochemical Co., Ltd. was used.
シリコーンオイルは、信越化学工業株式会社製のジメチルシリコーンオイルで、動粘度が40℃で20mm2/sのもの(DMSO−20と略記)と、350mm2/sのもの(DMSO−350と略記)を用いた。含窒素系界面活性剤は、ポリオキシエチレンアルキルアミン(POEAAと略記)と、アルキルアミンエチレンオキシド(AAEOと略記)付加体を用いた。また、フッ素系界面活性剤の代表として、ポリαオレフィン系グリースの拡散防止剤として有効なパーフルオロアルキルカルボン酸塩(PFACA塩と略記)を使用した。 Silicone oils are dimethyl silicone oils manufactured by Shin-Etsu Chemical Co., Ltd. and have a kinematic viscosity of 20 mm 2 / s (abbreviated as DMSO-20) and 350 mm 2 / s (abbreviated as DMSO-350) at 40 ° C. Was used. As the nitrogen-containing surfactant, polyoxyethylene alkylamine (abbreviated as POEAA) and an alkylamine ethylene oxide (abbreviated as AAEO) adduct were used. Further, as a representative of the fluorosurfactant, perfluoroalkylcarboxylate (abbreviated as PFACA salt) effective as a diffusion inhibitor for poly-α-olefin grease was used.
上記試料1と試料2は本発明例であり、シリコーンオイルと含窒素系界面活性剤を添加したフッ素グリース組成物である。試料3〜9は比較例であり、試料3はフッ素オイルをPTFEで増稠した通常のフッ素グリースである。比較例の試料4〜5は、40℃での動粘度が異なるシリコーンオイルのみを添加し、含窒素系界面活性剤を添加していないフッ素グリース組成物である。 Sample 1 and Sample 2 are examples of the present invention and are fluorine grease compositions to which silicone oil and a nitrogen-containing surfactant are added. Samples 3 to 9 are comparative examples, and sample 3 is a normal fluorine grease obtained by thickening fluorine oil with PTFE. Samples 4 to 5 of the comparative examples are fluorine grease compositions to which only silicone oils having different kinematic viscosities at 40 ° C. are added and no nitrogen-containing surfactant is added.
また、比較例の試料6〜7は、含窒素系界面活性剤のみを添加し、シリコーンオイルを添加していないフッ素グリース組成物である。比較例の試料8は、フッ素系界面活性剤(パーフルオロアルキルカルボン酸塩)のみを添加したものである。更に、比較例の試料9は、シリコーンオイルと上記フッ素系界面活性剤を添加したフッ素グリース組成物である。 Samples 6 to 7 of the comparative examples are fluorine grease compositions to which only a nitrogen-containing surfactant is added and no silicone oil is added. Sample 8 of the comparative example is obtained by adding only a fluorosurfactant (perfluoroalkylcarboxylate). Furthermore, sample 9 of the comparative example is a fluorine grease composition to which silicone oil and the above-mentioned fluorine-based surfactant are added.
上記試料1〜9のフッ素グリース組成物について、拡散防止性能を試験した。即ち、フッ素グリース組成物をラッピングペーパー(♯2000)に直径5mm、厚さ1mmの円柱状に塗布し、恒温槽内に50℃で24時間放置した後、円柱状のグリース外周部から外側に滲み出したオイルの端部までの平均距離を求め、得られた結果を下記表2に示した。 The fluorine grease compositions of Samples 1 to 9 were tested for diffusion prevention performance. That is, a fluorine grease composition is applied to wrapping paper (# 2000) in a cylindrical shape having a diameter of 5 mm and a thickness of 1 mm, left in a thermostatic bath at 50 ° C. for 24 hours, and then spreads from the outer periphery of the cylindrical grease to the outside. The average distance to the end of the extracted oil was determined, and the results obtained are shown in Table 2 below.
比較例の試料3は拡散防止剤が添加されていない通常のフッ素グリースであるから、この試料3の結果と比較することで、各フッ素グリース組成物の拡散防止効果を評価する。まず、本発明例である試料1、2のフッ素グリース組成物は、比較例の試料3に比べて、いずれも著しい拡散防止効果の向上を示した。 Since the sample 3 of the comparative example is a normal fluorine grease to which no diffusion inhibitor is added, the diffusion preventing effect of each fluorine grease composition is evaluated by comparing with the result of this sample 3. First, the fluorine grease compositions of Samples 1 and 2 which are examples of the present invention showed a significant improvement in the diffusion preventing effect as compared with Sample 3 of the comparative example.
一方、シリコーンオイルのみを添加した比較例の試料4〜5、フッ素系界面活性剤のみを配合した比較例の試料8、シリコーンオイルとフッ素系界面活性剤を配合した比較例の試料9については、比較例の試料3に比べて、いずれも拡散防止効果の向上が認められた。しかし、その拡散防止効果は僅かしか向上しておらず、従来要求されている性能には達していない。 On the other hand, with respect to Comparative Samples 4 to 5 in which only silicone oil was added, Comparative Sample 8 in which only a fluorosurfactant was blended, and Comparative Sample 9 in which silicone oil and a fluorosurfactant were blended, Compared with the sample 3 of the comparative example, the improvement of the diffusion preventing effect was recognized in all cases. However, the anti-diffusion effect has improved only slightly, and has not reached the performance required conventionally.
また、比較例の試料6〜7のフッ素グリース組成物は、本発明に用いる含窒素系界面活性剤のみを配合したものであるが、含窒素系界面活性剤のみを配合しても拡散防止効果はほとんど認められなかった。以上のことから、シリコーンオイルと含窒素系界面活性剤の併用により初めて、要求仕様を十分満たす極めて優れた拡散防止性能を有するフッ素グリースが得られることが分る。 In addition, the fluorine grease compositions of Comparative Samples 6 to 7 are those containing only the nitrogen-containing surfactant used in the present invention. Even if only the nitrogen-containing surfactant is added, the anti-diffusion effect is obtained. Was hardly recognized. From the above, it can be seen that a fluorine grease having an extremely excellent anti-diffusion performance that sufficiently satisfies the required specifications can be obtained only by the combined use of silicone oil and a nitrogen-containing surfactant.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007168468A JP5092117B2 (en) | 2007-06-27 | 2007-06-27 | Non-diffusible fluorine grease composition |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007168468A JP5092117B2 (en) | 2007-06-27 | 2007-06-27 | Non-diffusible fluorine grease composition |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2009007425A true JP2009007425A (en) | 2009-01-15 |
JP5092117B2 JP5092117B2 (en) | 2012-12-05 |
Family
ID=40322832
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2007168468A Expired - Fee Related JP5092117B2 (en) | 2007-06-27 | 2007-06-27 | Non-diffusible fluorine grease composition |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP5092117B2 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014113717A (en) * | 2012-12-07 | 2014-06-26 | Sumitomo Rubber Ind Ltd | Slide surface formation method in slide part of tire vulcanization container |
JP2015034206A (en) * | 2013-08-08 | 2015-02-19 | 協同油脂株式会社 | Grease composition |
JP2019111708A (en) * | 2017-12-22 | 2019-07-11 | 住友ゴム工業株式会社 | Method of applying fluorine grease |
KR102116747B1 (en) * | 2020-03-30 | 2020-06-02 | (주)씨엔루브 | Method for manufacturing baking equipment oven grease |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000109874A (en) * | 1998-10-05 | 2000-04-18 | Nippon Koyu:Kk | Non-diffusive fluorine grease composition |
JP2001354986A (en) * | 2000-06-12 | 2001-12-25 | Nok Kuluver Kk | Lubricating grease composition |
JP2003097571A (en) * | 2001-09-21 | 2003-04-03 | Nsk Ltd | Rolling bearing |
JP2003262228A (en) * | 2002-03-07 | 2003-09-19 | Nsk Ltd | Rolling device |
-
2007
- 2007-06-27 JP JP2007168468A patent/JP5092117B2/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000109874A (en) * | 1998-10-05 | 2000-04-18 | Nippon Koyu:Kk | Non-diffusive fluorine grease composition |
JP2001354986A (en) * | 2000-06-12 | 2001-12-25 | Nok Kuluver Kk | Lubricating grease composition |
JP2003097571A (en) * | 2001-09-21 | 2003-04-03 | Nsk Ltd | Rolling bearing |
JP2003262228A (en) * | 2002-03-07 | 2003-09-19 | Nsk Ltd | Rolling device |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014113717A (en) * | 2012-12-07 | 2014-06-26 | Sumitomo Rubber Ind Ltd | Slide surface formation method in slide part of tire vulcanization container |
JP2015034206A (en) * | 2013-08-08 | 2015-02-19 | 協同油脂株式会社 | Grease composition |
JP2019111708A (en) * | 2017-12-22 | 2019-07-11 | 住友ゴム工業株式会社 | Method of applying fluorine grease |
JP7041509B2 (en) | 2017-12-22 | 2022-03-24 | 住友ゴム工業株式会社 | Fluorine grease application method |
KR102116747B1 (en) * | 2020-03-30 | 2020-06-02 | (주)씨엔루브 | Method for manufacturing baking equipment oven grease |
Also Published As
Publication number | Publication date |
---|---|
JP5092117B2 (en) | 2012-12-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP4892282B2 (en) | Lubricating composition for electrical contacts | |
JP5035315B2 (en) | Perfluoropolyether oil composition | |
JP5092117B2 (en) | Non-diffusible fluorine grease composition | |
JP4421781B2 (en) | Grease composition for constant velocity joints | |
KR20030062260A (en) | Low torque grease composition | |
JP5652634B2 (en) | Grease composition for resin lubrication | |
WO2008004613A1 (en) | Grease composition and bearing | |
KR20140018369A (en) | Lubricating grease based on perfluoropolyether | |
JP2010195958A (en) | Lubricating composition for use in electric contact | |
JP4613530B2 (en) | Lubricating grease composition | |
JP4246707B2 (en) | lubricant | |
RU2581463C1 (en) | Grease | |
JPH10169657A (en) | Rolling device | |
RU2622400C1 (en) | Plastic lubrication | |
JP2007308578A (en) | Fluorine grease composition | |
CN112585253B (en) | Composition containing 1, 2-dichloro-3, 3, 3-trifluoropropene | |
JP2016147991A (en) | chain | |
JP6751833B2 (en) | Lubricant for chains | |
JP6281086B2 (en) | Non-diffusible fluorine-based lubricant composition | |
RU2569895C1 (en) | Synthetic oil composition for heat-stressed gas-turbine engines | |
WO2019049963A1 (en) | Grease composition and grease-enclosed roller bearing | |
JP6281085B2 (en) | Perfluoropolyether oil diffusion inhibitor and fluorine lubricant | |
JP2006046532A (en) | Slide screw | |
EP4269542A1 (en) | A lubricant using vegetable oil and having a self-generating friction film | |
US20220306963A1 (en) | Grease composition for metal-resin lubrication |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20090821 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20120418 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20120501 |
|
A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20120628 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20120821 |
|
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20120821 |
|
R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20150928 Year of fee payment: 3 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
LAPS | Cancellation because of no payment of annual fees |