JP2000239689A - Lubricating grease composition - Google Patents

Lubricating grease composition

Info

Publication number
JP2000239689A
JP2000239689A JP11359439A JP35943999A JP2000239689A JP 2000239689 A JP2000239689 A JP 2000239689A JP 11359439 A JP11359439 A JP 11359439A JP 35943999 A JP35943999 A JP 35943999A JP 2000239689 A JP2000239689 A JP 2000239689A
Authority
JP
Japan
Prior art keywords
oil
grease composition
base oil
lithium salt
fatty acid
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
Application number
JP11359439A
Other languages
Japanese (ja)
Other versions
JP4384318B2 (en
Inventor
Atsushi Shibayama
淳 柴山
Hiroshi Kimura
浩 木村
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kyodo Yushi Co Ltd
Original Assignee
Kyodo Yushi Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kyodo Yushi Co Ltd filed Critical Kyodo Yushi Co Ltd
Priority to JP35943999A priority Critical patent/JP4384318B2/en
Publication of JP2000239689A publication Critical patent/JP2000239689A/en
Application granted granted Critical
Publication of JP4384318B2 publication Critical patent/JP4384318B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To obtain a lubricating grease composition suitable for decreasing the noise of a bearing and increasing the life of it by compounding a base oil with a thickener containing lithium hydroxystearate and a lithium salt of a 6-11C fatty acid. SOLUTION: This composition contains a base oil and 5-40 mass % (based on the composition) thickener which comprises 5-95 mol% lithium hydroxystearate and 95-5 mol% lithium salt of a 6-11C fatty acid. The base oil is a carbonic ester compound, a synthetic ester oil (e.g. a polyol ester), a synthetic ether oil (e.g. an alkyl diphenyl ether), a synthetic hydrocarbon oil (e.g. a poly-α-olefin), a mineral oil (e.g, a paraffinic mineral oil) or the like, preferably contains 10 mass % or higher ester oil, and preferably has a kinematic viscosity (40 deg.C) of 5-20 mm2/s.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、潤滑グリース組成
物、特に玉軸受用グリースに関する。
The present invention relates to a lubricating grease composition, and more particularly to a grease for a ball bearing.

【従来の技術】従来、軸受、特にコンピュータのハード
ディスクやCD−ROM等の記録装置のスピンドルモー
タ用の玉軸受用グリースとしては、ジオクチルセバケー
ト、ペンタエリスリトールエステル等のエステル油を基
油とし、リチウムステアレート、リチウムヒドロキシス
テアレート等を増ちょう剤としたものが使用されてい
る。しかし、近年記録密度の増大に伴い、軸受精度の向
上や回転数の増加による使用温度の上昇等により、軸受
の音響寿命に不足が見られてきた。
2. Description of the Related Art Conventionally, greases for ball bearings, especially for ball bearings for spindle motors of recording devices such as hard disks and CD-ROMs of computers, are based on ester oils such as dioctyl sebacate and pentaerythritol ester. Those using thickeners such as stearate and lithium hydroxystearate are used. However, in recent years, with an increase in recording density, a shortage in acoustic life of the bearing has been observed due to an increase in operating temperature due to an improvement in bearing accuracy and an increase in the number of revolutions.

【0002】[0002]

【発明が解決しようとする課題】本発明の目的は、軸受
の音響特性の低騒音化及び長寿命化に適した潤滑グリー
ス組成物を提供することである。
SUMMARY OF THE INVENTION An object of the present invention is to provide a lubricating grease composition suitable for lowering the acoustic characteristics of a bearing and extending its life.

【0003】[0003]

【課題を解決するための手段】本発明は、基油と増ちょ
う剤を含むグリース組成物において、増ちょう剤が、
(a)ヒドロキシステアリン酸のリチウム塩と、(b)C6
14の脂肪酸のリチウム塩を含むことを特徴とする潤滑
グリース組成物を提供するものである。
SUMMARY OF THE INVENTION The present invention provides a grease composition containing a base oil and a thickener, wherein the thickener comprises:
(a) a lithium salt of hydroxystearic acid, (b) C 6 ~
There is provided a lubricating grease composition which comprises a lithium salt of a fatty acid of C 14.

【0004】[0004]

【発明の実施の形態】本発明者は、増ちょう剤として非
常に均質な繊維構造を有する石けんを使用することによ
り、本発明の目的が達成されることを見出した。このよ
うな、非常に均質な繊維構造を有する石けんは、(a)ヒ
ドロキシステアリン酸(例えば、12−ヒドロキシステ
アリン酸)のリチウム塩と、(b)C6 〜C14の脂肪酸の
リチウム塩を併用することにより形成される。ところ
で、ヒドロキシステアリン酸やC6 〜C14の脂肪酸とし
て一般に市販されているものの純度は様々であり、純度
の低いものは炭素原子数の異なる脂肪酸や不飽和の脂肪
酸等を含んでいる。目的の脂肪酸以外の脂肪酸の含有量
が多くなるとこれを使用して得られるグリースの性状が
不安定になる。そこで、本発明では、ヒドロキシステア
リン酸(例えば、12−ヒドロキシステアリン酸)、C
6〜C14の脂肪酸としていずれもその純度が80%(質量
%)以上のものを使用する。
DETAILED DESCRIPTION OF THE INVENTION The present inventors have found that the object of the present invention is achieved by using a soap having a very homogeneous fiber structure as a thickener. Such a soap having a very homogeneous fiber structure is obtained by combining (a) a lithium salt of hydroxystearic acid (eg, 12-hydroxystearic acid) with (b) a lithium salt of a C 6 -C 14 fatty acid. It is formed by doing. Incidentally, the purity of what is generally commercially available as hydroxystearic acid or fatty acid C 6 -C 14 are varied, those impure contains fatty acids of different fatty acids and unsaturation carbon atoms. If the content of fatty acids other than the target fatty acid increases, the properties of grease obtained using the same become unstable. Thus, in the present invention, hydroxystearic acid (eg, 12-hydroxystearic acid), C
As the 6 to C 14 fatty acids, those having a purity of 80% (mass%) or more are used.

【0005】ここで、成分(b) の脂肪酸のリチウム塩の
炭素原子数は6〜14である。炭素原子数が5以下の脂肪
酸のリチウム塩では基油に対する溶解性が低く、石けん
を溶解させるために260 ℃以上まで加温させる必要があ
るが、本発明に使用する基油には、引火点がこれ以下の
ものが多くあり製造時に危険を伴うため好ましくない。
炭素原子数が15以上の脂肪酸のリチウム塩は、主脂肪酸
であるヒドロキシステアリン酸のリチウム塩と性状が似
ており、混合した場合の効果があまり認められないた
め、あえて混合する必要性がなく、特に炭素原子数が20
を超えると、基油への溶解性が良過ぎるため、増ちょう
能力が劣り、目的のちょう度を得るために必要な石けん
量がヒドロキシステアリン酸のリチウム塩を100%使用し
た場合と比較して著しく多くなることからコスト的に好
ましくない。
The fatty acid lithium salt of the component (b) has 6 to 14 carbon atoms. Lithium salts of fatty acids having 5 or less carbon atoms have low solubility in base oils and must be heated to 260 ° C. or higher to dissolve soap. However, many of them are less than this, which is not preferable because it involves danger during production.
Lithium salts of fatty acids having 15 or more carbon atoms are similar in property to the lithium salts of hydroxystearic acid, which is the main fatty acid, and the effect when mixed is not recognized so much, there is no need to dare to mix, Especially 20 carbon atoms
If it exceeds, because the solubility in the base oil is too good, the thickening ability is inferior, the amount of soap required to obtain the desired consistency is compared to the case where 100% of the lithium salt of hydroxystearic acid is used. This is not preferable in terms of cost because it is extremely large.

【0006】(a) ヒドロキシステアリン酸のリチウム塩
と、(b) C6 からC14の脂肪酸のリチウム塩のモル比
は、好ましくは5〜95:95〜5、さらに好ましくは10〜9
5:90〜5である。基油の40℃の動粘度は、好ましくは5
〜200mm2/s、さらに好ましくは10〜100mm2/s である。
本発明の潤滑グリース組成物の基油としては、炭酸エス
テル化合物、ポリオールエステル油等のエステル系合成
油、アルキルジフェニルエーテル等のエーテル系合成
油、ポリアルファ−オレフィン等の合成炭化水素油、パ
ラフィン系鉱油等の鉱物油が挙げられる。
The molar ratio of (a) the lithium salt of hydroxystearic acid to (b) the lithium salt of a C 6 to C 14 fatty acid is preferably from 5 to 95:95 to 5, more preferably from 10 to 9
5: 90-5. The kinematic viscosity of the base oil at 40 ° C. is preferably 5
200200 mm 2 / s, more preferably 10-100 mm 2 / s.
Examples of the base oil of the lubricating grease composition of the present invention include carbonate compounds, ester synthetic oils such as polyol ester oils, ether synthetic oils such as alkyl diphenyl ether, synthetic hydrocarbon oils such as polyalpha-olefins, and paraffinic mineral oils. And other mineral oils.

【0007】基油として特に好ましいものは、10質量%
以上、さらに好ましくは50質量%以上のエステル油を含
有するものである。増ちょう剤の含有量は、組成物全体
に対して好ましくは、5〜40質量%、さらに好ましくは
7〜20質量%である。
A particularly preferred base oil is 10% by mass.
Above, more preferably 50% by mass or more of ester oil. The content of the thickener is preferably 5 to 40% by mass, more preferably 7 to 20% by mass, based on the whole composition.

【0008】以下、実施例により本発明を具体的に説明
する。 実施例1 基油として、ペンタエリスリトールエステル油(40℃:33
mm2/s)を使用し、以下のように基油中で脂肪酸と水酸化
リチウムを反応させてグリース組成物(各200g)を調
製した。脂肪酸量は10質量%、水酸化リチウム量は、け
ん化価実測値の5%増しとした。脂肪酸は純度80%以上
のものを使用した。 a)基油と脂肪酸を混合したビーカーを約80℃まで加温
し、基油中に溶解する。 b)水酸化リチウムと5倍の蒸留水を混合したビーカー
を約80℃まで加温する。 c)aにbを一気に投入し、約5分反応させる。 d)反応後加温を行い、石けんを油に溶解させ(最高温
度 235℃)、室温までそのまま冷却し、3本ロールミル
に1回通し混練して、所定のグリースを得た(クリアラ
ンス10〜20μm)。
Hereinafter, the present invention will be described in detail with reference to examples. Example 1 As a base oil, pentaerythritol ester oil (40 ° C .: 33
mm 2 / s), a fatty acid and lithium hydroxide were reacted in a base oil as follows to prepare a grease composition (200 g each). The amount of fatty acid was increased by 10% by mass, and the amount of lithium hydroxide was increased by 5% from the measured saponification value. Fatty acids having a purity of 80% or more were used. a) A beaker containing a mixture of a base oil and a fatty acid is heated to about 80 ° C. and dissolved in the base oil. b) Warm a beaker containing a mixture of lithium hydroxide and 5 times distilled water to about 80 ° C. c) Charge b into a at a stretch and let it react for about 5 minutes. d) Warming is performed after the reaction, the soap is dissolved in oil (maximum temperature 235 ° C.), cooled as it is to room temperature, and kneaded once through a three-roll mill to obtain a predetermined grease (clearance 10 to 20 μm). ).

【0009】実施例2 基油として、ペンタエリスリトールエステル油(40℃:3
3mm2/s)を使用し、以下のようにグリース組成物(各200
g)を調製した。石けん量は10質量%とした。 a)基油とリチウム石けんを一つのビーカに秤取り、 2
35℃まで加温する。 b)石けんを油に溶解後、室温までそのまま冷却し、3
本ロールミルに1回通し混練して、所定のグリースを得
た(クリアランス10〜20μm)。
Example 2 As a base oil, pentaerythritol ester oil (40 ° C .: 3
3mm 2 / s) and use the grease composition (200
g) was prepared. The amount of soap was 10% by mass. a) Weigh the base oil and lithium soap into one beaker,
Heat to 35 ° C. b) After dissolving the soap in oil, cool it to room temperature,
The mixture was passed through the roll mill once and kneaded to obtain a predetermined grease (clearance: 10 to 20 μm).

【0010】音響寿命試験方法 下記条件で一定時間運転させた後、アンデロン試験機
(菅原研究所製:AD-SN-4)を用いて、アンデロン量(音
量)及びノイズの多少を点数化し、標準品(比較例1の
試料10、比較例2の試料11、または参考例の試料16)と
比較した。 (1)試験条件 軸受形式:608VV 試験温度:100℃ 回転数 :1800rpm 試験時間:500h グリース充填量:0.35ml(軸受空間容積の約40%) (2)アンデロン試験(アンデロン量とノイズを測定) 回転数 :1800rpm 試験時間:120秒 評価 標準品に対して、以下の規準で判定した。 A:標準品の1.1倍を越えるもの B:標準品の0.9〜1.1倍のもの C:標準品のO.9倍未満のもの
[0010] Sound life test method After operating for a certain period of time under the following conditions, an Anderon tester
Using (AD-SN-4 manufactured by Sugawara Laboratories), the amount of anderon (volume) and the degree of noise were scored to obtain standard products (Sample 10 of Comparative Example 1, Sample 11 of Comparative Example 2, or Reference Example). Sample 16) was compared. (1) Test conditions Bearing type: 608 VV Test temperature: 100 ° C Rotation speed: 1800 rpm Test time: 500 h Grease filling amount: 0.35 ml (about 40% of bearing space volume) (2) Anderon test (measures anderon amount and noise) ) Number of revolutions: 1800 rpm Test time: 120 seconds Evaluation A standard product was judged according to the following criteria. A: More than 1.1 times the standard product B: 0.9 to 1.1 times the standard product C: Less than 0.9 times the standard product

【0011】[0011]

【石けん繊維の長さ、幅の確認方法】石けん繊維の長
さ、幅の確認は、電子顕微鏡(株式会社明石製作所製;
LEM-2000)にて測定した。得られたグリースをワセリン
にてサンプルを5〜20倍に希釈し、これを、電子顕微鏡
用の金属メッシュ上に塗布する。次に、溶剤(n-ヘキサ
ン等)を入れたシャーレに金属メッシュを置き、グリー
スより油成分を除去する。溶剤中より金属メッシュを取
り出し、乾燥した後、電子顕微鏡にセットし、石けん繊
維を観察する。測定倍率は6000倍とし、一視野の主流を
占める代表的大きさの繊維5点の長さ及び幅を測定し、
その平均を求める。結果を以下の表に示す。
[How to check the length and width of soap fiber] To check the length and width of soap fiber, use an electron microscope (Akashi Seisakusho Co., Ltd .;
LEM-2000). The obtained grease is diluted with petrolatum to 5 to 20 times the sample, and this is applied on a metal mesh for an electron microscope. Next, a metal mesh is placed on a petri dish containing a solvent (such as n-hexane), and oil components are removed from the grease. The metal mesh is taken out of the solvent, dried, set on an electron microscope, and the soap fiber is observed. The measurement magnification is 6000 times, and the length and width of five points of fibers of a typical size that occupy the mainstream of one field of view are measured,
Find the average. The results are shown in the table below.

【0012】[0012]

【表1】 [Table 1]

【0013】[0013]

【表2】 混和ちょう度、滴点及び音響寿命の欄の「-」は、試験
していないことを意味する。
[Table 2] The "-" in the columns of compatibility penetration, dropping point and acoustic life means that the test was not performed.

【0014】実施例1及び比較例1に使用したヒドロキ
システアリン酸は12−ヒドロキシステアリン酸(純度8
5%)である。また、使用した他の脂肪酸の純度は90%以上
である。石けん繊維の大きさは、試料1〜9、11につ
いては、試料10と比較して細く短かかったが、試料1
2は試料10と同等であった。
The hydroxystearic acid used in Example 1 and Comparative Example 1 was 12-hydroxystearic acid (purity 8
5%). The purity of the other fatty acids used is 90% or more. As for the size of the soap fiber, the samples 1 to 9 and 11 were thinner and shorter than the sample 10;
2 was equivalent to sample 10.

【0015】[0015]

【表3】 [Table 3]

【0016】[0016]

【表4】 混和ちょう度及び音響寿命の欄の「-」は、試験してい
ないことを意味する。
[Table 4] "-" In the columns of the penetration and acoustic life means that the test was not performed.

【0017】実施例2及び比較例2に使用したヒドロキ
システアリン酸リチウムは12−ヒドロキシステアリン
酸リチウム(純度85%)である。また、使用した他の脂肪
酸の純度は90%以上である。参考例の試料16は、純度
約70%の12−ヒドロキシステアリン酸リチウムを使用
し、基油として、ペンタエリスリトールエステル油とジ
エステル油を80:20の重量比率で使用した。基油の
動粘度は40℃で26.0mm2/s であり、グリース組成物の滴
点は190 ℃であった。石けん繊維の大きさは、試料1〜
10については、試料11と比較して細く短かかった
が、試料13、14、16は試料11と同等であり、試
料15は試料11と比較して太く、長かった。
The lithium hydroxystearate used in Example 2 and Comparative Example 2 is lithium 12-hydroxystearate (85% purity). The purity of the other fatty acids used is 90% or more. Sample 16 of the reference example used lithium 12-hydroxystearate having a purity of about 70%, and used pentaerythritol ester oil and diester oil at a weight ratio of 80:20 as base oils. The kinematic viscosity of the base oil was 26.0 mm 2 / s at 40 ° C, and the drop point of the grease composition was 190 ° C. The size of the soap fiber is from sample 1
Sample 10 was thinner and shorter than sample 11, but samples 13, 14, and 16 were equivalent to sample 11, and sample 15 was thicker and longer than sample 11.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 FI テーマコート゛(参考) C10N 40:02 50:10 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C10N 40:02 50:10

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】 基油と増ちょう剤を含むグリース組成物
において、増ちょう剤が、(a)ヒドロキシステアリン酸
のリチウム塩と、(b)C6 〜C14の脂肪酸のリチウム塩
を含むことを特徴とする潤滑グリース組成物。
1. A grease composition comprising a base oil and a thickener, wherein the thickener comprises (a) a lithium salt of hydroxystearic acid and (b) a lithium salt of a C 6 -C 14 fatty acid. A lubricating grease composition comprising:
【請求項2】 (a) ヒドロキシステアリン酸のリチウム
塩と、(b) C6〜C1 4の脂肪酸のリチウム塩のモル比
が、5〜95:95〜5である請求項1記載の潤滑グリース組
成物。
2. A lithium salt (a) of hydroxystearic acid, the molar ratio of the lithium salt of (b) C 6 ~C 1 4 fatty acid, 5-95: 95-5 lubricating of claim 1, wherein Grease composition.
【請求項3】 基油の40℃の動粘度が5〜200mm2/sであ
る請求項1または2記載の潤滑グリース組成物。
3. The lubricating grease composition according to claim 1, wherein the kinematic viscosity at 40 ° C. of the base oil is 5 to 200 mm 2 / s.
【請求項4】 基油が、10質量%以上のエステル油を含
有する請求項1〜3のいずれか1項記載の潤滑グリース
組成物。
4. The lubricating grease composition according to claim 1, wherein the base oil contains at least 10% by mass of an ester oil.
【請求項5】 増ちょう剤の含有量が、組成物全体に対
して5〜40質量%である請求項1〜4のいずれか1項記
載の潤滑グリース組成物。
5. The lubricating grease composition according to claim 1, wherein the content of the thickener is 5 to 40% by mass based on the whole composition.
JP35943999A 1998-12-22 1999-12-17 Lubricating grease composition Expired - Lifetime JP4384318B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP10-365085 1998-12-22
JP36508598 1998-12-22
JP35943999A JP4384318B2 (en) 1998-12-22 1999-12-17 Lubricating grease composition

Publications (2)

Publication Number Publication Date
JP2000239689A true JP2000239689A (en) 2000-09-05
JP4384318B2 JP4384318B2 (en) 2009-12-16

Family

ID=26580969

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Country Status (1)

Country Link
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JP2005213329A (en) * 2004-01-28 2005-08-11 Kyodo Yushi Co Ltd Grease composition
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US20160201726A1 (en) * 2012-12-04 2016-07-14 Kyodo Yushi Co., Ltd. Rolling device
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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KR102613104B1 (en) * 2015-05-01 2023-12-12 세이코 인스트루 가부시키가이샤 Grease for rolling bearing of information recording and reproducing apparatus, rolling bearing, rolling bearing device, and information recording and reproducing apparatus

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