JP7212359B2 - Base oil diffusion inhibitor and grease containing it - Google Patents
Base oil diffusion inhibitor and grease containing it Download PDFInfo
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Description
本発明は、グリースの基油の拡散を防止するために用いる基油拡散防止剤に関し、特にシリコーンオイルを基油とするグリースの基油の拡散を防止するために用いる基油拡散防止剤に関するものである。 TECHNICAL FIELD The present invention relates to a base oil diffusion inhibitor used to prevent diffusion of the base oil of grease, and more particularly to a base oil diffusion inhibitor used to prevent diffusion of the base oil of grease having silicone oil as its base oil. is.
各種機器の急速な高性能化及び小型化に伴って、その機械的な回転部や摺動部等に使用されるグリースに対して、従来よりも優れた特性が求められている。たとえば、小型化された各種機構部、モーター類、各種ベアリング類、接点類又はスイッチ類等に使用するグリースでは、特に、耐熱性、低温安定性及び軽トルク性等の特性が求められている。 With the rapid improvement in performance and miniaturization of various types of equipment, greases used in mechanical rotating parts, sliding parts, etc. are required to have better properties than ever before. For example, greases used in miniaturized mechanisms, motors, bearings, contacts, switches, etc. are particularly required to have properties such as heat resistance, low-temperature stability, and light torque.
これらの特性を満足するために、エステル系又はポリアルファオレフィン系等の合成潤滑油を基油として、ウレア系又は石鹸系等の増ちょう剤を添加したグリースが市販されている。しかしながら、かかる市販のグリースは、基油が比較的低粘度であるため、グリース塗布後に、時間の経過と共に基油が塗布面から拡散してしまうという問題があった。特に、小型化された機器に適用されるグリースでは、基油の拡散は防止されるべき事項である。このため、基油拡散防止剤として、フルオロアルキルシラン化合物を用いることが記載されている（特許文献１）。また、パーフルオロポリアルキルエーテル油を基油とし、この基油に基油拡散防止剤としてパーフルオロイソプロポキシアルキルシラン化合物を添加することが記載されている（特許文献２）。 In order to satisfy these characteristics, greases are commercially available which contain a synthetic lubricating oil such as an ester or polyalphaolefin as a base oil and a thickener such as a urea or soap. However, since the base oil of such commercially available grease has a relatively low viscosity, there is a problem that the base oil diffuses from the applied surface over time after the grease is applied. In particular, in greases that are applied to miniaturized equipment, diffusion of the base oil should be prevented. For this reason, it is described that a fluoroalkylsilane compound is used as a base oil diffusion inhibitor (Patent Document 1). Moreover, it is described that a perfluoropolyalkyl ether oil is used as a base oil, and a perfluoroisopropoxyalkylsilane compound is added to this base oil as a base oil diffusion inhibitor (Patent Document 2).
しかしながら、年々小型化が進む機器においては、フルオロアルキルシラン化合物又はパーフルオロイソプロポキシアルキルシラン化合物よりなる基油拡散防止剤では、その効果が不十分であった。 However, in devices that are becoming smaller year by year, the effect of base oil diffusion inhibitors comprising fluoroalkylsilane compounds or perfluoroisopropoxyalkylsilane compounds is insufficient.
本発明の課題は、基油拡散防止能のより向上した基油拡散防止剤を提供することにある。 An object of the present invention is to provide a base oil diffusion inhibitor with improved base oil diffusion prevention ability.
本発明は、特許文献１及び２に記載されているシラン化合物とは異なり、加水分解性シリル基に特定の連結基を介して特定のパーフルオロアルキレンエーテル基が結合されてなるシラン化合物を採用することにより、上記課題を解決したものである。すなわち、本発明は、下記一般式（１）で表される、分子量１０００以下のシラン化合物を含む基油拡散防止剤に関するものである。
Ｚ－ＰＦＰＥ－Ｘ－Ｓｉ（ＯＲ1）p（Ｒ2）q・・・（１）
一般式（１）中のＺは、炭素数１～６のフロオロアルキル基であり、特に好ましくはパーフルオロアルキル基である。また、Ｚは、［（Ｒ2）q（Ｒ1Ｏ）pＳｉ－Ｘ］基であってもよく、Ｒ1、Ｒ2、Ｘ、ｐ及びｑの意味は後述するとおりである。ＰＦＰＥは、［（ＯＣ6Ｆ12）a－（ＯＣ5Ｆ10）b－（ＯＣ4Ｆ8）c－（ＯＣ3Ｆ6）d－（ＯＣ2Ｆ4）e－（ＯＣＦ2）f］基を表し、ａ、ｂ、ｃ、ｄ、ｅ及びｆは、それぞれ独立して０以上１０以下の整数であって、ａ、ｂ、ｃ、ｄ、ｅ及びｆの和が１以上となるものである。なお、ａ、ｂ、ｃ、ｄ、ｅ及びｆを付した各パーフルオロオキシアルキレン基の存在順序は任意である。Ｘは、アミド基、カルバメート基、アルキレン基及びオキシアルキレン基から選ばれた連結基を表す。Ｒ1及びＲ2は独立に低級アルキル基であり、好ましくは炭素数１～３のアルキル基である。ｐは１～３の整数を、ｑは０～２の整数を表し、ｐとｑの和は３である。
Unlike the silane compounds described in Patent Documents 1 and 2, the present invention employs a silane compound in which a specific perfluoroalkylene ether group is bonded to a hydrolyzable silyl group via a specific linking group. Thus, the above problem is solved. That is, the present invention relates to a base oil diffusion inhibitor containing a silane compound having a molecular weight of 1000 or less represented by the following general formula (1).
Z-PFPE-X-Si(OR 1 ) p (R 2 ) q (1)
Z in the general formula (1) is a fluoroalkyl group having 1 to 6 carbon atoms, preferably a perfluoroalkyl group. Z may also be a [(R 2 ) q (R 1 O) p Si—X] group, and the meanings of R 1 , R 2 , X, p and q are as described below. PFPE is [( OC6F12 ) a- ( OC5F10 ) b- ( OC4F8 ) c- ( OC3F6 ) d- ( OC2F4 ) e- ( OCF2 ) f ] a, b, c, d, e, and f are each independently an integer of 0 or more and 10 or less, and the sum of a, b, c, d, e, and f is 1 or more is. The order in which the perfluorooxyalkylene groups with a, b, c, d, e and f are present is arbitrary. X represents a linking group selected from an amide group, carbamate group, alkylene group and oxyalkylene group. R 1 and R 2 are independently lower alkyl groups, preferably alkyl groups having 1 to 3 carbon atoms. p is an integer of 1 to 3, q is an integer of 0 to 2, and the sum of p and q is 3.
本発明に用いるシラン化合物は、上記一般式（１）で表されるものであり、分子量は１０００以下である。分子量が１０００を超えると、フルオロアルキル基やパーフルオロオキシアルキレン基の鎖長が長くなり、基油との相溶性が悪くなり基油拡散防止効果が低下する傾向となる。具体的には、以下のシラン化合物が好適である。
（ア）Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣ2Ｈ5）3
（イ）Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（ウ）Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－ＣＨ2Ｏ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（エ）Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－ＣＨ2ＯＣ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（オ）Ｃ3Ｆ7－（ＯＣＦ2ＣＦ2ＣＦ2）3－ＯＣ2Ｆ4－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（カ）Ｃ3Ｆ7－［ＯＣＦ（ＣＦ3）ＣＦ2］2－ＯＣＦ（ＣＦ3）Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（キ）Ｃ3Ｆ7－［ＯＣＦ（ＣＦ3）ＣＦ2］3－ＯＣＦ（ＣＦ3）Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣ2Ｈ5）3
（ク）Ｃ3Ｆ7－［ＯＣＦ（ＣＦ3）ＣＦ2］2－ＯＣＦ（ＣＦ3）ＣＨ2Ｏ（ＣＨ2）3－Ｓｉ（ＯＣ2Ｈ5）3
（ケ）Ｃ3Ｆ7－［ＯＣＦ（ＣＦ3）ＣＦ2］3－ＯＣＦ（ＣＦ3）ＣＨ2Ｏ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（コ）Ｃ3Ｆ7－［ＯＣＦ（ＣＦ3）ＣＦ2］3－ＯＣＦ（ＣＦ3）ＣＨ2ＯＣ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（サ）（Ｈ3ＣＯ）3Ｓｉ－（ＣＨ2）3ＮＨＣ（Ｏ）ＣＦ2Ｏ－（ＣＦ2ＣＦ2Ｏ）2－ＯＣＦ2－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（シ）（Ｈ3ＣＯ）3Ｓｉ－（ＣＨ2）3ＮＨＣ（Ｏ）ＣＦ2Ｏ－（ＣＦ2ＣＦ2Ｏ）2－（ＯＣＦ2）2－ＯＣＦ2－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（ス）（Ｈ3ＣＯ）3Ｓｉ－（ＣＨ2）3ＮＨＣ（Ｏ）ＯＣＨ2ＣＦ2Ｏ－（ＣＦ2ＣＦ2Ｏ）2－（ＯＣＦ2）2－ＯＣＦ2ＣＨ2Ｏ－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
なお、本発明に用いるシラン化合物は、加水分解により、一部縮合体となっていてもよい。
The silane compound used in the present invention is represented by the general formula (1) and has a molecular weight of 1000 or less. If the molecular weight exceeds 1,000, the chain length of the fluoroalkyl group or perfluorooxyalkylene group becomes long, the compatibility with the base oil is deteriorated, and the anti-diffusion effect of the base oil tends to decrease. Specifically, the following silane compounds are suitable.
(a) C4F9-( OCF2CF2 ) 2 - OCF2 - C(O)NH( CH2 ) 3 - Si ( OC2H5 ) 3
(a) C4F9- ( OCF2CF2 ) 2 - OCF2 - C(O)NH( CH2 ) 3 - Si(OCH3) 3
(c) C4F9- ( OCF2CF2 ) 2 -OCF2 - CH2O ( CH2 ) 3 - Si( OCH3 ) 3
(d) C4F9- ( OCF2CF2 ) 2 - OCF2 - CH2OC ( O)NH( CH2 ) 3 - Si(OCH3) 3
(e) C3F7- ( OCF2CF2CF2 ) 3 - OC2F4 - C ( O)NH( CH2 ) 3 - Si( OCH3 ) 3
(f) C3F7- [OCF( CF3 )CF2] 2 - OCF( CF3 )C(O)NH( CH2 ) 3 - Si( OCH3 ) 3
(g) C3F7- [OCF( CF3 )CF2] 3 - OCF( CF3 )C(O)NH( CH2 ) 3 - Si ( OC2H5 ) 3
(h) C3F7- [OCF( CF3 )CF2] 2 -OCF( CF3 ) CH2O ( CH2 ) 3 - Si ( OC2H5 ) 3
(i) C3F7- [OCF( CF3 )CF2] 3 -OCF( CF3 ) CH2O ( CH2 ) 3 - Si ( OCH3 ) 3
(ko) C3F7- [OCF( CF3 )CF2] 3 - OCF( CF3 ) CH2OC ( O)NH( CH2 ) 3 - Si(OCH3) 3
(k) (H 3 CO) 3 Si—(CH 2 ) 3 NHC(O)CF 2 O—(CF 2 CF 2 O) 2 —OCF 2 —C(O)NH(CH 2 ) 3 —Si(OCH 3 ) 3
(C) (H 3 CO) 3 Si—(CH 2 ) 3 NHC(O)CF 2 O—(CF 2 CF 2 O) 2 —(OCF 2 ) 2 —OCF 2 —C(O)NH(CH 2 ) 3 -Si(OCH 3 ) 3
(S) (H 3 CO) 3 Si—(CH 2 ) 3 NHC(O)OCH 2 CF 2 O—(CF 2 CF 2 O) 2 —(OCF 2 ) 2 —OCF 2 CH 2 OC(O )NH( CH2 ) 3 - Si(OCH3) 3
The silane compound used in the present invention may be partially condensed by hydrolysis.
本発明に係るシラン化合物を含む基油拡散防止剤を、基油及び増ちょう剤に添加してグリースとして用いられる。基油としては、シリコーン油、エステル油、炭化水素系合成油、鉱物油又はフッ素系オイル等の従来公知の基油が用いられる。特に、本発明においては、シリコーン油を基油とするのが好ましい。本発明に用いるシラン化合物及びシリコーン油は、いずれも珪素元素を含む化合物であって、相溶性に優れており、本発明に係る基油拡散防止剤の効果が向上するからである。増ちょう剤としても、リチウム石けん又はカルシウム石けん等の金属石けん系増ちょう剤並びにウレア、ＰＴＦＥ又はベントン等の非石けん系増ちょう剤等の従来公知の増ちょう剤が用いられる。 A base oil diffusion inhibitor containing the silane compound according to the present invention is added to a base oil and a thickener to be used as a grease. As the base oil, a conventionally known base oil such as silicone oil, ester oil, hydrocarbon synthetic oil, mineral oil or fluorine oil is used. In particular, in the present invention, it is preferable to use silicone oil as the base oil. This is because both the silane compound and the silicone oil used in the present invention are compounds containing a silicon element and have excellent compatibility, which improves the effect of the base oil diffusion inhibitor according to the present invention. As the thickener, conventionally known thickeners such as metallic soap-based thickeners such as lithium soap or calcium soap and non-soap thickeners such as urea, PTFE or bentone are used.
また、本発明に係るシラン化合物を含む基油拡散防止剤を、市販グリースに添加して、グリースを調製してもよい。市販グリースとしては、ＫＳ－６０９（信越化学工業株式会社製）又はＫＳ－６５０Ｎ（信越化学工業株式会社製）等のシリコーン系グリース、スミテック３３１（住鉱潤滑剤株式会社製）等のポリαオレフィン系グリース、スミテックＳＧ４０２（住鉱潤滑剤株式会社製）等のエステル系グリース並びにデムナムグリース（ダイキン工業株式会社製）、バリエルタ（ＮＯＫクリューバー株式会社製）又はスミテック（住鉱潤滑剤株式会社製）等のフッ素系グリースが用いられる。 Also, the base oil diffusion inhibitor containing the silane compound according to the present invention may be added to commercially available grease to prepare grease. Commercially available greases include silicone greases such as KS-609 (manufactured by Shin-Etsu Chemical Co., Ltd.) and KS-650N (manufactured by Shin-Etsu Chemical Co., Ltd.), and poly-α-olefins such as Sumitec 331 (manufactured by Sumiko Lubricant Co., Ltd.). Ester-based grease such as Sumitec SG402 (manufactured by Sumiko Lubricant Co., Ltd.), Demnum grease (manufactured by Daikin Industries, Ltd.), Varierta (manufactured by NOK Klüber Co., Ltd.) or Sumitec (manufactured by Sumiko Lubricant Co., Ltd.) ) or the like is used.
本発明に係る基油拡散防止剤は、グリース総量に対して、０．１～１０重量％程度含有され、特に０．５～５重量％程度含有させるのが好ましい。 The base oil diffusion inhibitor according to the present invention is contained in an amount of about 0.1 to 10% by weight, preferably about 0.5 to 5% by weight, based on the total amount of the grease.
本発明に係る基油拡散防止剤は、シリコーン油等の基油の拡散を防止しうる効果を奏する。したがって、本発明に係る基油拡散防止剤を含有するグリースは、小型化された機器に適用されても、長期に亙って良好な潤滑性能を与えるという効果を奏する。 The base oil diffusion inhibitor according to the present invention has an effect of preventing diffusion of base oil such as silicone oil. Therefore, the grease containing the base oil diffusion inhibitor according to the present invention has the effect of providing good lubricating performance over a long period of time even when applied to downsized equipment.
実施例１
市販シリコーングリース（信越化学工業株式会社製、ＫＳ－６０９）に、下記化学式で表されるシラン化合物（分子量７６５）よりなる基油拡散防止剤を３質量％添加した後、均一に攪拌してグリースを得た。
Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣ2Ｈ5）3
Example 1
After adding 3% by mass of a base oil diffusion inhibitor consisting of a silane compound (molecular weight 765) represented by the following chemical formula to commercially available silicone grease (KS-609, manufactured by Shin-Etsu Chemical Co., Ltd.), the grease is uniformly stirred. got
C4F9-( OCF2CF2 ) 2 - OCF2 - C(O)NH( CH2 ) 3 - Si ( OC2H5 ) 3
実施例２
基油拡散防止剤の添加量を１質量％にした他は、実施例１と同様にしてグリースを得た。
Example 2
A grease was obtained in the same manner as in Example 1, except that the amount of the base oil diffusion inhibitor added was 1% by mass.
実施例３
基油拡散防止剤の添加量を０．１質量％にした他は、実施例１と同様にしてグリースを得た。
Example 3
A grease was obtained in the same manner as in Example 1, except that the amount of the base oil diffusion inhibitor added was 0.1% by mass.
実施例４
市販シリコーングリースに代えて、市販ポリαオレフィングリース（住鉱潤滑剤株式会社製、スミテック３３１）を用いた他は、実施例１と同様にしてグリースを得た。
Example 4
A grease was obtained in the same manner as in Example 1, except that a commercially available poly-α-olefin grease (Sumitec 331, manufactured by Sumiko Lubricant Co., Ltd.) was used instead of the commercially available silicone grease.
実施例５
基油拡散防止剤の添加量を１質量％にした他は、実施例４と同様にしてグリースを得た。
Example 5
A grease was obtained in the same manner as in Example 4, except that the amount of the base oil diffusion inhibitor added was 1% by mass.
実施例６
実施例１で用いたシラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表されるシラン化合物（分子量７７９）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＣＦ2ＣＨ2－Ｏ－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣ2Ｈ5）3
Example 6
The procedure of Example 1 was repeated except that instead of the base oil diffusion inhibitor made of the silane compound used in Example 1, a base oil diffusion inhibitor made of a silane compound (molecular weight: 779) represented by the following chemical formula was used. got the grease.
C4F9- ( OCF2CF2 ) 2 - CF2CH2 -OC(O)NH( CH2 ) 3 - Si ( OC2H5 ) 3
実施例７
実施例１で用いたシラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表されるシラン化合物（分子量８４４）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
（Ｈ5Ｃ2Ｏ）3Ｓｉ－（ＣＨ2）3ＮＨＣ（Ｏ）－ＣＦ2－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－Ｃ（Ｏ）ＮＨ－（ＣＨ2）3－Ｓｉ（ＯＣ2Ｈ5）3
Example 7
The procedure of Example 1 was repeated except that instead of the base oil diffusion inhibitor made of the silane compound used in Example 1, a base oil diffusion inhibitor made of a silane compound (molecular weight: 844) represented by the following chemical formula was used. got the grease.
(H 5 C 2 O) 3 Si—(CH 2 ) 3 NHC(O)—CF 2 —(OCF 2 CF 2 ) 2 —OCF 2 —C(O)NH—(CH 2 ) 3 —Si(OC 2 H5 ) 3
実施例８
実施例１で用いたシラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表されるシラン化合物（分子量７２１）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＣＦ2ＣＨ2－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
Example 8
The procedure of Example 1 was repeated except that instead of the base oil diffusion inhibitor made of the silane compound used in Example 1, a base oil diffusion inhibitor made of a silane compound (molecular weight: 721) represented by the following chemical formula was used. got the grease.
C4F9- ( OCF2CF2 ) 2 - CF2CH2 - C(O)NH( CH2 ) 3 - Si( OCH3 ) 3
比較例１
シラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表される化合物（分子量５４８）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
Ｃ4Ｆ9－（ＯＣＦ2ＣＦ2）2－ＯＣＦ2－ＣＨ2ＯＨ
Comparative example 1
A grease was obtained in the same manner as in Example 1, except that a base oil diffusion inhibitor made of a compound represented by the following chemical formula (molecular weight: 548) was used instead of the base oil diffusion inhibitor made of a silane compound.
C4F9- ( OCF2CF2 ) 2 - OCF2 - CH2OH
比較例２
基油拡散防止剤の添加量を１質量％にした他は、比較例１と同様にしてグリースを得た。
Comparative example 2
A grease was obtained in the same manner as in Comparative Example 1, except that the amount of the base oil diffusion inhibitor added was 1% by mass.
比較例３
シラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表される化合物（分子量約１５００）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
ＨＯＣＨ2ＣＦ2Ｏ（ＣＦ2ＣＦ2Ｏ）m（ＣＦ2Ｏ）nＣＦ2ＣＨ2ＯＨ
（式中、ｍは約６であり、ｎは約１０である。）
Comparative example 3
A grease was obtained in the same manner as in Example 1 except that instead of the base oil diffusion inhibitor made of a silane compound, a base oil diffusion inhibitor made of a compound represented by the following chemical formula (molecular weight: about 1500) was used.
HOCH2CF2O ( CF2CF2O ) m ( CF2O ) nCF2CH2OH
(Where m is about 6 and n is about 10.)
比較例４
基油拡散防止剤の添加量を１質量％にした他は、比較例３と同様にしてグリースを得た。
Comparative example 4
A grease was obtained in the same manner as in Comparative Example 3, except that the amount of the base oil diffusion inhibitor added was 1% by mass.
比較例５
シラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表される化合物（分子量約３９００）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
Ｃ3Ｆ7－（ＯＣＦ2ＣＦ2ＣＦ2）l－ＯＣＦ2ＣＦ2ＣＨ2Ｏ－Ｃ（Ｏ）ＮＨ（ＣＨ2）3－Ｓｉ（ＯＣＨ3）3
（式中、ｌは約２１である。）
Comparative example 5
A grease was obtained in the same manner as in Example 1 except that instead of the base oil diffusion inhibitor made of a silane compound, a base oil diffusion inhibitor made of a compound represented by the following chemical formula (molecular weight: about 3900) was used.
C3F7- ( OCF2CF2CF2 ) 1 - OCF2CF2CH2OC ( O)NH( CH2 ) 3 - Si ( OCH3 ) 3
(Where l is about 21.)
比較例６
シラン化合物よりなる基油拡散防止剤に代えて、下記化学式で表される化合物（分子量６５２）よりなる基油拡散防止剤を用いた他は、実施例１と同様にしてグリースを得た。
ＣＦ3－（ＣＦ2）7ＣＨ2ＣＨ2－Ｓｉ（ＯｉＰｒ）3
（式中、ｉＰｒはイソプロピル基である。）
Comparative example 6
A grease was obtained in the same manner as in Example 1, except that a base oil diffusion inhibitor made of a compound represented by the following chemical formula (molecular weight: 652) was used instead of the base oil diffusion inhibitor made of a silane compound.
CF3- ( CF2) 7CH2CH2 - Si (OiPr) 3
(Wherein, iPr is an isopropyl group.)
比較例７
市販シリコーングリース（信越化学工業株式会社製、ＫＳ－６０９）のみとした。
Comparative example 7
Only commercially available silicone grease (KS-609, manufactured by Shin-Etsu Chemical Co., Ltd.) was used.
比較例８
市販ポリαオレフィングリース（住鉱潤滑剤株式会社製、スミテック３３１）のみとした。
Comparative example 8
Only commercially available poly-α-olefin grease (Sumitec 331 manufactured by Sumiko Lubricant Co., Ltd.) was used.
［基油拡散試験］
実施例１～８及び比較例１～８で得られた各グリースを、ポリエステルフィルム（ソマブラックフィルム Ｒ１００ＭＤ ソマール株式会社製）表面に、直径６ｍｍで高さ１ｍｍの円柱状に塗布した。そして、８０℃の恒温器に入れて促進試験を行い、２４時間後の基油の拡散状態を評価した。図１に示すように、基油は塗布したグリースの径方向に拡散するので、基油の直径（Ａｍｍ）を測定した。そして、拡散幅（ｍｍ）＝Ａ－６を求めた。この結果を表１に示した。
[Base oil diffusion test]
Each of the greases obtained in Examples 1 to 8 and Comparative Examples 1 to 8 was applied to the surface of a polyester film (Somablack film R100MD manufactured by Somar Co., Ltd.) in the form of a cylinder having a diameter of 6 mm and a height of 1 mm. Then, an accelerated test was performed by placing it in a thermostatic chamber at 80° C., and the diffusion state of the base oil was evaluated after 24 hours. As shown in FIG. 1, the diameter (Amm) of the base oil was measured because the base oil spreads in the radial direction of the applied grease. Then, diffusion width (mm)=A-6 was obtained. The results are shown in Table 1.
［表１］
━━━━━━━━━━━━━━━━
拡散幅
━━━━━━━━━━━━━━━━
実施例１ ０ｍｍ
実施例２ ０ｍｍ
実施例３ ４ｍｍ
実施例４ ０ｍｍ
実施例５ ０ｍｍ
実施例６ ０ｍｍ
実施例７ ０ｍｍ
実施例８ ０ｍｍ
比較例１ １１ｍｍ
比較例２ １３ｍｍ
比較例３ １０ｍｍ
比較例４ １５ｍｍ
比較例５ ２０ｍｍ
比較例６ １１ｍｍ
比較例７ ２１ｍｍ
比較例８ ５０ｍｍ
━━━━━━━━━━━━━━━━
[Table 1]
━━━━━━━━━━━━━━━━
diffusion width
━━━━━━━━━━━━━━━━
Example 1 0mm
Example 2 0mm
Example 3 4mm
Example 4 0mm
Example 5 0 mm
Example 6 0mm
Example 7 0mm
Example 8 0mm
Comparative example 1 11mm
Comparative example 2 13mm
Comparative example 3 10mm
Comparative example 4 15mm
Comparative example 5 20mm
Comparative example 6 11mm
Comparative example 7 21mm
Comparative example 8 50mm
━━━━━━━━━━━━━━━━
表１の結果から明らかなように、実施例に係る各グリースは、比較例に係る各グリースに比べて、基油の拡散が顕著に防止されていることが分かる。 As is clear from the results in Table 1, the respective greases according to the examples significantly prevent the diffusion of the base oil compared to the respective greases according to the comparative examples.
Claims (4)
Ｚ－ＰＦＰＥ－Ｘ－Ｓｉ（ＯＲ1）p（Ｒ2）q・・・（１）
｛式中：
Ｚは、炭素数１～６のフルオロアルキル基又は［（Ｒ2）q（Ｒ1Ｏ）pＳｉ－Ｘ］基を表し、；
ＰＦＰＥは、［（ＯＣ6Ｆ12）a－（ＯＣ5Ｆ10）b－（ＯＣ4Ｆ8）c－（ＯＣ3Ｆ6）d－（ＯＣ2Ｆ4）e－（ＯＣＦ2）f］基を表し［但し、ａ、ｂ、ｃ、ｄ、ｅ及びｆは、それぞれ独立して０以上１０以下の整数であって、ａ、ｂ、ｃ、ｄ、ｅ及びｆの和は、１以上である。なお、ａ、ｂ、ｃ、ｄ、ｅ及びｆを付した各パーフルオロオキシアルキレン基の存在順序は任意である。］、
Ｘは、アミド基、カルバメート基、アルキレン基及びオキシアルキレン基から選ばれた連結基を表し、
Ｒ1及びＲ2は独立に低級アルキル基を表し、ｐは１～３の整数を表し、ｑは０～２の整数を表し、ｐとｑの和は３である。｝ A base oil diffusion inhibitor containing a silane compound having a molecular weight of 1000 or less, represented by the general formula (1).
Z-PFPE-X-Si(OR 1 ) p (R 2 ) q (1)
{In the formula:
Z represents a fluoroalkyl group having 1 to 6 carbon atoms or a [(R 2 ) q (R 1 O) p Si—X] group;
PFPE is [( OC6F12 ) a- ( OC5F10 ) b- ( OC4F8 ) c- ( OC3F6 ) d- ( OC2F4 ) e- ( OCF2 ) f ] [wherein a, b, c, d, e and f are each independently integers of 0 or more and 10 or less, and the sum of a, b, c, d, e and f is 1 or more is. The order in which the perfluorooxyalkylene groups with a, b, c, d, e and f are present is arbitrary. ],
X represents a linking group selected from an amide group, a carbamate group, an alkylene group and an oxyalkylene group;
R 1 and R 2 independently represent a lower alkyl group, p represents an integer of 1 to 3, q represents an integer of 0 to 2, and the sum of p and q is 3. }
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| JP2005247998A (en) | 2004-03-04 | 2005-09-15 | Kanto Kasei Kogyo Kk | Silicone grease composition |
| JP2007308578A (en) | 2006-05-18 | 2007-11-29 | Sumikou Junkatsuzai Kk | Fluorine grease composition |
| JP2008201901A (en) | 2007-02-20 | 2008-09-04 | Nippon Koyu Ltd | Non-diffusing lubricant composition and method for preventing diffusion of base oil |
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| JP2540393B2 (en) * | 1991-05-15 | 1996-10-02 | 株式会社日本礦油 | Non-diffusible lubricating composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005247998A (en) | 2004-03-04 | 2005-09-15 | Kanto Kasei Kogyo Kk | Silicone grease composition |
| JP2007308578A (en) | 2006-05-18 | 2007-11-29 | Sumikou Junkatsuzai Kk | Fluorine grease composition |
| JP2008201901A (en) | 2007-02-20 | 2008-09-04 | Nippon Koyu Ltd | Non-diffusing lubricant composition and method for preventing diffusion of base oil |
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