JP2008297519A - Grease base oil diffusion preventing agent - Google Patents
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本発明は、グリース中の基油の拡散を防止し、且つグリースの着色が起こりにくいグリース基油拡散防止剤組成物、及び各種精密機器類の機械的な回転部や摺動部等に好適に用いることができる前記グリース基油拡散防止剤組成物を配合したグリースに関する。 The present invention is suitable for a grease base oil diffusion inhibitor composition that prevents the diffusion of base oil in grease and hardly causes coloring of grease, and mechanical rotating parts and sliding parts of various precision instruments. The present invention relates to a grease containing the grease base oil diffusion inhibitor composition that can be used.
各種機器の急速な高性能化、小型化に伴って、その機械的な回転部、摺動部に使用されているグリースに対しても従来よりも優れた特性が求められている。例えば、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、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、軽トルク性等が求められている。 With the rapid performance improvement and miniaturization of various devices, the grease used for the mechanical rotating part and sliding part is required to have characteristics superior to those of conventional ones. For example, greases used for various miniaturized mechanisms, motors, various bearings, contacts, switches, and the like are particularly required to have heat resistance, low temperature stability, light torque, and the like.
これらの性能を満足するために、市販のグリースにはウレア系又は石鹸系等の増稠剤を、低粘度の合成潤滑油からなる基油中に分散させている。しかしながら、このような従来のグリースでは、基油として前述のような合成潤滑油を使用しているため、グリース塗布後にグリース成分中の油分もしくは油状添加物が、時間の経過とともに塗布面から拡散（滲出）してしまうという問題がある。 In order to satisfy these performances, in a commercially available grease, a thickener such as urea or soap is dispersed in a base oil composed of a synthetic lubricating oil having a low viscosity. However, in such a conventional grease, since the synthetic lubricating oil as described above is used as the base oil, the oil or oily additive in the grease component diffuses from the coated surface as time passes ( There is a problem of exudation).
この基油の拡散を防止する方法として、例えば、疎水性基としてパーフルオロカーボンチェーンをもち、かつ親水性基としてポリオキシエチレンをもつフッ素系界面活性剤を合成潤滑油を基油とするグリースに添加する方法が提案されている（例えば、特許文献１参照。）。しかしながら、この方法では基油拡散を防止することはできるが、経時によりグリースが着色しやすいという新たな問題が生じ、基油拡散防止効果があり、かつ経時的にグリースが着色しない添加剤が求められている。さらに、パーフルオロアルキル基含有ポリオキシエチレン系化合物とパーフルオロアルキル基含有アルコール化合物とを混合して用いると、前記拡散防止、非着色性には効果があるものの、グリースに配合した際に、前記のパーフルオロアルキル基含有ポリオキシエチレン系化合物が蒸発しやすく、例えば、プロジェクターランプのレンズ周辺に使用されている部材に用いると、曇りが発生する問題点を有していた。 As a method of preventing the diffusion of this base oil, for example, a fluorosurfactant having a perfluorocarbon chain as a hydrophobic group and polyoxyethylene as a hydrophilic group is added to grease based on a synthetic lubricating oil. A method has been proposed (for example, see Patent Document 1). However, although this method can prevent base oil diffusion, there is a new problem that the grease is likely to be colored over time, and an additive that has an effect of preventing base oil diffusion and does not color the grease over time is desired. It has been. Furthermore, when a perfluoroalkyl group-containing polyoxyethylene compound and a perfluoroalkyl group-containing alcohol compound are used in combination, the diffusion prevention and non-coloring properties are effective, but when blended in grease, The peroxyalkyl group-containing polyoxyethylene compound tends to evaporate. For example, when it is used for a member used around a lens of a projector lamp, there is a problem that fogging occurs.
したがって、本発明の課題は、非着色性であり、且つ基油拡散防止効果があり、これに加えて、蒸発量が少ないグリース基油拡散防止剤を提供することである。 Accordingly, an object of the present invention is to provide a grease base oil diffusion preventing agent that is non-coloring and has a base oil diffusion preventing effect, and in addition, has a small amount of evaporation.
本発明者等は、上記課題を解決すべく鋭意検討を行ったところ、下記一般式（１）を用いたグリース基油拡散防止剤が、前記課題が解決できることを見出し、本発明を完成した。 The inventors of the present invention have intensively studied to solve the above-mentioned problems. As a result, they found that a grease base oil diffusion inhibitor using the following general formula (1) can solve the above-mentioned problems, and completed the present invention.
すなわち本発明は、下記一般式（１）で表されるパーフルオロアルキル基含有ポリオキシアルキレン系化合物（Ａ）を含有することを特徴とするグリース基油拡散防止剤、 That is, the present invention comprises a grease base oil diffusion inhibitor comprising a perfluoroalkyl group-containing polyoxyalkylene compound (A) represented by the following general formula (1):
本発明によれば、拡散防止効果があり、かつ経時的に着色せず、更に、グリースとして用いたときに、添加剤の蒸発量の少ないグリース基油拡散防止剤、及びこれを配合したグリースを提供することができる。 According to the present invention, there is provided a grease base oil diffusion preventing agent that has a diffusion preventing effect, does not color with time, and has a small amount of evaporation of the additive when used as a grease, and a grease containing the same. Can be provided.
本発明で用いる前記一般式（１）は、具体的には、下記一般式（２）又は（３）で表されるものである。 The general formula (1) used in the present invention is specifically represented by the following general formula (2) or (3).
（一般式（２）中のＸが炭素数１〜４のヒドロキシアルキル基または炭素数１〜５のアシル基、ｐは０〜５０、ｑは０〜３０の繰り返し単位数をそれぞれ表し、ｐ＋ｑは３以上でありまた一般式（３）中のＲｆは炭素数１〜３０のパーフルオロアルキル基、Ｒは、水素原子、炭素数１〜５のアルキル基、ｒは３〜２５の繰り返し単位数を表す。） (X in the general formula (2) represents a hydroxyalkyl group having 1 to 4 carbon atoms or an acyl group having 1 to 5 carbon atoms, p represents 0 to 50, q represents the number of repeating units of 0 to 30, and p + q represents 3 or more, and Rf in the general formula (3) is a perfluoroalkyl group having 1 to 30 carbon atoms, R is a hydrogen atom, an alkyl group having 1 to 5 carbon atoms, and r is the number of repeating units of 3 to 25. To express.)
前記一般式（２）の中でも、平均分子量１０００以上であるものが、添加剤が蒸発しにくいことから好ましく、平均分子量５０００以下であるものが基油拡散を防止する点から好ましく、更に、１０００〜３０００であるものが特に好ましい。 Among the general formula (2), those having an average molecular weight of 1000 or more are preferable because the additive is difficult to evaporate, and those having an average molecular weight of 5000 or less are preferable from the viewpoint of preventing base oil diffusion. Particularly preferred is 3000.
更に、前記一般式（２）の中でも、Ｘがヒドロキシメチル基または炭素数１〜５のアルキルカルボニルオキシメチル基であるものが好ましい。これらの具体例としては、Ｘが、炭素数１〜５のアルキルカルボニルオキシメチル基であるものとしては、ソルベイ ソレクシス社製フルオロリンクＬ１０Ｈ等が挙げられ、また、Ｘがヒドロキシメチル基であるものとしては、ソルベイ ソレクシス社製のフルオロリンクＤ１０Ｈ、フルオロリンクＤが挙げられ、ヒドロキシエチル基を有するものとしてはフルオロリンクＥ１０Ｈ、フルオロリンクＥ等が挙げられる。 Furthermore, among the said General formula (2), what is X is a hydroxymethyl group or a C1-C5 alkylcarbonyloxymethyl group is preferable. Specific examples of these are those in which X is an alkylcarbonyloxymethyl group having 1 to 5 carbon atoms, such as Fluorolink L10H manufactured by Solvay Solexis, and X is a hydroxymethyl group. Examples thereof include Fluorolink D10H and Fluorolink D manufactured by Solvay Solexis. Examples of those having a hydroxyethyl group include Fluorolink E10H and Fluorolink E.
前記前記一般式（２）で表される化合物の中でも、化合物の両末端に水酸基を有する化合物が低蒸発量という観点から好ましい。 Among the compounds represented by the general formula (2), a compound having hydroxyl groups at both ends of the compound is preferable from the viewpoint of low evaporation.
前記一般式（３）の中でも、平均分子量５００以上であるものが、添加剤が蒸発しにくいことから好ましく、平均分子量６０００以下であるものが基油拡散を防止する点から好ましく、更に、８００〜３０００であるものが特に好ましい。 Among the general formula (3), those having an average molecular weight of 500 or more are preferable because the additive is difficult to evaporate, and those having an average molecular weight of 6000 or less are preferable from the viewpoint of preventing base oil diffusion, and more preferably 800 to Particularly preferred is 3000.
更に、前記一般式（３）で表される化合物の中でも、ｒが、６〜２０であり、Ｒｆが−ＣＦ３または−Ｃ２Ｆ５である化合物が、低蒸発量という観点から好ましい。 Furthermore, among the compounds represented by the general formula (3), a compound in which r is 6 to 20 and Rf is —CF 3 or —C 2 F 5 is preferable from the viewpoint of low evaporation.
前記一般式（２）で表される化合物と一般式（３）で表される化合物は、それぞれ単独で使用してもよいし、混合して使用してもよい。 The compound represented by the general formula (2) and the compound represented by the general formula (3) may be used alone or in combination.
本発明のグリース基油拡散防止剤を適用するグリースとしては、種々のグリースを用いることが出来、特に制限されるものではない。例えば本発明のグリースに用いることができる増稠剤としては、金属石鹸系、複合石鹸系などの石鹸系増稠剤、又はウレア系増稠剤などが挙げられる。また、本発明のグリースに用いることができる基油としては、例えば、ポリαオレフィン油、エチレンαオレフィンコオリゴマー油、シリコン油、ジエステル油等の合成潤滑油が挙げられる。 As the grease to which the grease base oil diffusion inhibitor of the present invention is applied, various greases can be used and are not particularly limited. For example, examples of the thickener that can be used in the grease of the present invention include soap-based thickeners such as metal soaps and composite soaps, or urea-based thickeners. Examples of the base oil that can be used in the grease of the present invention include synthetic lubricating oils such as poly α-olefin oil, ethylene α-olefin co-oligomer oil, silicon oil, and diester oil.
本発明のグリースは、本発明のグリース基油拡散防止剤を配合したものであり、その配合方法としては特に限定されるものではない。例えば、予め、グリース基油拡散防止剤を基油に該グリース基油拡散防止剤組成物を混合し更に増稠剤を配合し、均一化する方法、基油と増稠剤との混合物に後から該グリース基油拡散防止剤を添加し均一化する方法、基油にグリース基油拡散防止剤組成物と増稠剤とを一括で配合して均一に混合する方法等が挙げられる。 The grease of the present invention is formulated with the grease base oil diffusion inhibitor of the present invention, and the blending method is not particularly limited. For example, a method of previously mixing a grease base oil diffusion inhibitor composition with a grease base oil diffusion inhibitor composition and further blending a thickener and homogenizing the grease base oil diffusion inhibitor, and then mixing the base oil with the thickener The grease base oil diffusion inhibitor is added and homogenized, and the base oil is mixed with the grease base oil diffusion inhibitor composition and the thickener and mixed uniformly.
このとき、均一化のために３０〜６０℃に加温することも可能である。また、グリース中のグリース基油拡散防止剤の配合量としては、目的とする非拡散性と非着色性、低蒸発製の要求レベルに応じて適宜選択されるものである。得られるグリースの全重量を１００重量％とするとき、該グリース中に、本発明のグリース基油拡散防止剤を０．１〜１０重量％含有していることが、非拡散性と非着色性の効果が発現しやすく、特に１〜５重量％含有していることが好ましい。 At this time, it is also possible to heat to 30 to 60 ° C. for homogenization. Further, the blending amount of the grease base oil diffusion inhibitor in the grease is appropriately selected according to the desired level of non-diffusibility, non-coloration, and low evaporation. When the total weight of the obtained grease is 100% by weight, the grease contains the grease base oil diffusion preventing agent of the present invention in an amount of 0.1 to 10% by weight. This effect is easy to express, and it is particularly preferable to contain 1 to 5% by weight.
本発明のグリースの用途としては特に限定されるものではなく、特に各種精密機器類の機械的な回転部や摺動部等に好適に用いることができ、特に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、スイッチ類等に使用することが出来、グリースが本来有する耐熱性や軽トルク性を損なうことなく、基油の拡散を防止し且つ経時着色しにくく、且つ、使用する部材周辺を曇らせないものである。 The application of the grease of the present invention is not particularly limited, and can be suitably used particularly for mechanical rotating parts and sliding parts of various precision instruments. Particularly, various miniaturized mechanism parts and motors can be used. It can be used for various types of bearings, various bearings, contacts, switches, etc., prevents the base oil from diffusing and does not easily color over time, without compromising the heat resistance and light torque properties inherent in grease. The surroundings of the member to be made are not fogged.
次に、本発明を実施例及び比較例により更に詳細に説明する。
＜実施例１＞
下記構造式（Ｉ）で表され化合物（Ａ−１）〔平均分子量１５００、Ｘがヒドロキシメチル基、ｐが６、ｑが１０である。〕１．０重量部とコスモグリース ダイナッマックスＮｏ．１（コスモ石油ルブリカンツ(株)製）１００重量部添加し、均一に混合して、グリース（１Ａ）を得た。
＜実施例２＞
実施例１において、用いる化合物（Ａ−１）を化合物（Ａ−２）〔平均分子量２０００、Ｘがヒドロキシメチル基、ｐが８、ｑが１３である。〕としたこと以外は実施例１と同様にして、グリース（２Ａ）を得た。
＜実施例３＞
実施例１において、用いる化合物（Ａ−１）を化合物（Ａ−２）〔平均分子量１５００、Ｘがヒドロキシエチル基、ｐが３、ｑが１５である。〕としたこと以外は実施例１と同様にして、グリース（３Ａ）を得た。
＜実施例４＞
実施例１において、用いる化合物（Ａ−１）を化合物（Ａ−４）〔平均分子量２０００、Ｘがヒドロキシエチル基、ｐが８、ｑが１３である。〕としたこと以外は実施例１と同様にして、グリース（４Ａ）を得た。
＜実施例５＞
実施例１において、用いる化合物（Ａ−１）を化合物（Ａ−５）〔平均分子量１５００、Ｘがメチルカルボニルオキシメチル基、ｐが２、ｑが１４である。〕としたこと以外は実施例１と同様にして、グリース（５Ａ）を得た。
＜実施例６＞
実施例１において、用いる化合物（Ａ−１）を一般式（３）で表される化合物（Ｂ−１）〔平均分子量１１２０、Ｒｆが−ＣＦ３、ｒが６〕としたこと以外は実施例１と同様にして、グリース（１Ｂ）を得た。
＜実施例７＞
実施例１において、用いる化合物（Ａ−１）を一般式（３）で表される化合物（Ｂ−２）〔平均分子量１４００、Ｒｆが−Ｃ２Ｆ５、ｒが６〕としたこと以外は実施例１と同様にして、グリース（２Ｂ）を得た。
＜実施例８＞
実施例１において、用いる化合物（Ａ−１）を一般式（３）で表される化合物（Ｂ−３）〔平均分子量４７００、Ｒｆが−Ｃ２Ｆ５、ｒが２０〕としたこと以外は実施例１と同様にして、グリース（３Ｂ）を得た。
＜比較例１＞
前記化合物（Ａ−１）をメガファックＦ−２６０（大日本インキ化学工業製パーフルオロアルキル基含有ポリオキシエチレン系化合物）を用いた以外は実施例１と同様にして、グリース（１Ｃ）を得た。
＜比較例２＞
前記化合物（Ａ−１）を下記一般式（４）で表されるフォンブリンＹ−０６（ソルベイ ソレクシス製パーフルオロアルキル基含有ポリオキシエチレン系化合物）を用いた以外は実施例１と同様にして、グリース（２Ｃ）を得た。
Next, the present invention will be described in more detail with reference to examples and comparative examples.
<Example 1>
Compound (A-1) represented by the following structural formula (I) [average molecular weight 1500, X is a hydroxymethyl group, p is 6, and q is 10. ] 1.0 part by weight and Cosmo Grease Dynamax No. 100 parts by weight of 1 (manufactured by Cosmo Oil Lubricants Co., Ltd.) was added and mixed uniformly to obtain grease (1A).
<Example 2>
In Example 1, the compound (A-1) used is the compound (A-2) [average molecular weight 2000, X is a hydroxymethyl group, p is 8, and q is 13. Except for the above, a grease (2A) was obtained in the same manner as in Example 1.
<Example 3>
In Example 1, the compound (A-1) used is the compound (A-2) [average molecular weight 1500, X is a hydroxyethyl group, p is 3, and q is 15. Except for the above, a grease (3A) was obtained in the same manner as in Example 1.
<Example 4>
In Example 1, the compound (A-1) used is the compound (A-4) [average molecular weight 2000, X is a hydroxyethyl group, p is 8, and q is 13. Except for the above, a grease (4A) was obtained in the same manner as in Example 1.
<Example 5>
In Example 1, the compound (A-1) used is the compound (A-5) [average molecular weight 1500, X is a methylcarbonyloxymethyl group, p is 2, and q is 14. Except for the above, a grease (5A) was obtained in the same manner as in Example 1.
<Example 6>
In Example 1, except that the compound (A-1) used is the compound (B-1) represented by the general formula (3) [average molecular weight 1120, Rf is —CF 3 , r is 6]. In the same manner as in No. 1, grease (1B) was obtained.
<Example 7>
In Example 1, except that the compound (A-1) used is the compound (B-2) represented by the general formula (3) [average molecular weight 1400, Rf is —C 2 F 5 , r is 6]. In the same manner as in Example 1, a grease (2B) was obtained.
<Example 8>
In Example 1, except that the compound (A-1) used is the compound (B-3) represented by the general formula (3) [average molecular weight 4700, Rf is —C 2 F 5 , r is 20]. In the same manner as in Example 1, a grease (3B) was obtained.
<Comparative Example 1>
Grease (1C) was obtained in the same manner as in Example 1 except that Megafac F-260 (Dainippon Ink Chemicals Co., Ltd. perfluoroalkyl group-containing polyoxyethylene compound) was used as the compound (A-1). It was.
<Comparative example 2>
Example 1 was used except that Fomblin Y-06 (a perfluoroalkyl group-containing polyoxyethylene compound manufactured by Solvay Solexis) represented by the following general formula (4) was used as the compound (A-1). A grease (2C) was obtained.
＜比較例３＞
前記化合物（Ａ−１）を前記一般式（４）で表されるフォンブリンＹ−２５（ソルベイ ソレクシス製パーフルオロアルキル基含有ポリオキシエチレン系化合物）を用いた以外は実施例１と同様にして、グリース（３Ｃ）を得た。
<Comparative Example 3>
Except for using Fomblin Y-25 (a peroxyalkyl group-containing polyoxyethylene compound manufactured by Solvay Solexis) represented by the general formula (4) as the compound (A-1), the same as in Example 1. A grease (3C) was obtained.
＜比較例４＞
前記化合物（Ａ−１）を前記一般式（５）で表されるパーフルオロアルキル基含有ポリオキシエチレン系化合物（５）を用いた以外は実施例１と同様にして、グリース（４Ｃ）を得た。
<Comparative Example 4>
A grease (4C) was obtained in the same manner as in Example 1 except that the peroxyalkyl group-containing polyoxyethylene compound (5) represented by the general formula (5) was used as the compound (A-1). It was.
ＣｍＦ２ｍ＋１−（ＣＨ２ＣＨ２Ｏ）ｙ−Ｈ （５）
（ここで、ｍ＝６〜１０、ｙは平均６．５の分布品）
C m F 2m + 1 - ( CH 2 CH 2 O) y -H (5)
(Where m = 6 to 10 and y is a distribution product with an average of 6.5)
試験例１〜８及び比較試験例１〜４
実施例１〜８、比較例１〜３で得られたグリースを用いて、下記試験方法によって、拡散性と着色性を評価し、その結果を表１に示した。
Test Examples 1-8 and Comparative Test Examples 1-4
Using the greases obtained in Examples 1 to 8 and Comparative Examples 1 to 3, diffusibility and colorability were evaluated by the following test methods, and the results are shown in Table 1.
図１に基づいて試験方法を説明する。 The test method will be described with reference to FIG.
まずグリース１を直径１０ｍｍ、高さ０．２ｍｍの円柱形になるようにスリガラス板（１００ｍｍ×１００ｍｍ）２の粗面の上に塗布する。そして、恒温器中に入れて８０℃の条件で促進試験を行い、２４時間後の基油の拡散状態を評価した。即ち、円柱形に塗布したグリース１から基油が拡散した場合、図１に示すように、スリガラス板２の粗面が半透明状態になった部分３が確認される。この半透明状態になった部分の幅を拡散幅とした。促進試験後、基油の拡散が全く確認されなかった場合を○、拡散幅が１５ｍｍ以下の場合は△、拡散幅が１５ｍｍを越えた場合を×とした。 First, grease 1 is applied on the rough surface of a ground glass plate (100 mm × 100 mm) 2 so as to form a cylindrical shape having a diameter of 10 mm and a height of 0.2 mm. And it put in the thermostat and the acceleration test was done on 80 degreeC conditions, and the spreading | diffusion state of the base oil 24 hours after was evaluated. That is, when the base oil diffuses from the grease 1 applied in a cylindrical shape, a portion 3 where the rough surface of the ground glass plate 2 is translucent is confirmed as shown in FIG. The width of this translucent portion was defined as the diffusion width. After the acceleration test, the case where no diffusion of the base oil was confirmed was indicated by ◯, the case where the diffusion width was 15 mm or less, Δ, and the case where the diffusion width exceeded 15 mm, ×.
また、上述の促進試験後の外観を観察し、着色性を評価した。促進試験後のグリースを、添加剤を添加する前のグリースの色と比較して、全く着色が認められない場合を○とし、やや変色が認められた場合を△とし、明らかに変色した場合を×とした。 Moreover, the external appearance after the above-mentioned acceleration test was observed and coloring property was evaluated. The grease after the accelerated test is compared with the color of the grease before the additive is added. X.
添加剤の蒸発量（重量％）
アルミシャーレに添加剤試料１ｇを量り採りも１０７．５℃の乾燥機中で２時間放置したあとの重量を測定した。その際の減量を、測定前の質量に対する重量％で表し、これを蒸発量とした。なお、本発明における好ましい蒸発量としては、３０重量％以下、更に好ましくは２０重量％以下である。
Evaporation amount of additive (wt%)
An additive sample (1 g) was weighed in an aluminum petri dish and weighed after being left in a dryer at 107.5 ° C. for 2 hours. The weight loss at that time was expressed as% by weight relative to the mass before measurement, and this was defined as the amount of evaporation. In addition, as a preferable evaporation amount in this invention, it is 30 weight% or less, More preferably, it is 20 weight% or less.
表１に示したように、試験例１〜８のグリースは、基油拡散防止効果があり、かつ非着色性に優れるものであった。 As shown in Table 1, the greases of Test Examples 1 to 8 had a base oil diffusion preventing effect and were excellent in non-coloring properties.
本発明のグリース基油拡散防止剤組成物を配合したグリースは、各種精密機器類の機械的な回転部や摺動部等に好適に用いることができる。 The grease containing the grease base oil diffusion inhibitor composition of the present invention can be suitably used for mechanical rotating parts and sliding parts of various precision instruments.
１…グリース、２…スリガラス板、３…拡散部分。 DESCRIPTION OF SYMBOLS 1 ... Grease, 2 ... Ground glass board, 3 ... Diffusion part.
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| JP2014231548A (en) * | 2013-05-28 | 2014-12-11 | 住鉱潤滑剤株式会社 | Perfluoropolyether oil diffusion preventive and fluorine-based lubricant |
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