JPH05504369A - Lubricating grease composition - Google Patents

Lubricating grease composition

Info

Publication number
JPH05504369A
JPH05504369A JP3504602A JP50460291A JPH05504369A JP H05504369 A JPH05504369 A JP H05504369A JP 3504602 A JP3504602 A JP 3504602A JP 50460291 A JP50460291 A JP 50460291A JP H05504369 A JPH05504369 A JP H05504369A
Authority
JP
Japan
Prior art keywords
lithium
grease composition
grease
acid
composition
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
JP3504602A
Other languages
Japanese (ja)
Other versions
JP2964165B2 (en
Inventor
マダー，ボルフガング
グルン，ゲオルグ
Original Assignee
ボルフガンク　フランツ　エベルハルト　マダー
ゲオルク　グリューン
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Filing date
Publication date
Application filed by ボルフガンク　フランツ　エベルハルト　マダー, ゲオルク　グリューン filed Critical ボルフガンク　フランツ　エベルハルト　マダー
Publication of JPH05504369A publication Critical patent/JPH05504369A/en
Application granted granted Critical
Publication of JP2964165B2 publication Critical patent/JP2964165B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M113/00—Lubricating compositions characterised by the thickening agent being an inorganic material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
    • C10M117/04—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen containing hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/06—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having more than one carboxyl group bound to an acyclic carbon atom or cycloaliphatic carbon atom
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/08—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to a carbon atom of a six-membered aromatic ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/10—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having more than one carboxyl group bound to a carbon atom of a six-membered aromatic ring
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    • C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M133/12—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to a carbon atom of a six-membered aromatic ring
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
    • C10M135/18—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond thiocarbamic type, e.g. containing the groups
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    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/06—Well-defined aromatic compounds
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
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    • C10M2203/1025—Aliphatic fractions used as base material
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Abstract

(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。 (57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 潤滑性グリース組成物 本発明は、潤滑性グリース組成物に関し、より詳しくはリチウム石ケンで増粘し たグリース組成物に関する。[Detailed description of the invention] Lubricating grease composition The present invention relates to lubricating grease compositions, and more particularly to lubricating grease compositions thickened with lithium soap. The present invention relates to a grease composition.

リチウム石ケングリースは周知であり、多数の自動車用及び工業用用途、例えば ヘアリング、歯車及び軸継手に用いられている。リチウム石ケングリース及び特 にリチウム石ケンコンプレックス（ｃ　ｏｍｐ　Ｉ　ｅ　ｘ）グリースは、屡々 高温の用途に好まれるが、このグリースは、約１２０　’Ｃを越える温度では寿 命が限られているという欠点がある。それは油がグリースから分離する（ブリー ド）傾向があり、従ってグリースを頻繁に再施用する必要があるがらである。Lithium soap grease is well known and used in numerous automotive and industrial applications, e.g. Used in hair rings, gears, and shaft couplings. Lithium soap grease and special Lithium soap complex (comp ix) grease is often Although preferred for high temperature applications, this grease has a limited lifetime at temperatures above approximately 120'C. The drawback is that your life is limited. It separates the oil from the grease (bleeding). c) There is a tendency for grease to be reapplied frequently.

本発明は、高温度で長時間の寿命を有するリチウムコンプレックスグリースを提 供する。より詳しくは、本発明は、大部分の割合の潤滑用基油、増粘量のリチウ ム石ケンコンプレンクス及び有効量の、金属がモリブデン、タングステン、バナ ジウム、ニオブ及びタンタルから選ばれる有機金属化合物を含む潤滑用グリース 組成物を提供する。The present invention provides a lithium complex grease with long service life at high temperatures. provide More specifically, the present invention comprises a major proportion of lubricating base oil, a thickening amount of lithium The mineral complex and effective amounts of metals such as molybdenum, tungsten, and Lubricating grease containing an organometallic compound selected from dium, niobium and tantalum A composition is provided.

本発明のグリースは、高温での寿命が大いに改善されるという利点を持つ。この 改善は、約１２０〜１６０　’Ｃで特に明らかである。The grease of the invention has the advantage that its life at high temperatures is greatly improved. this The improvement is particularly evident at about 120-160'C.

このグリースは他のリチウム石ケン含有グリースに較べて油をブリードする傾向 が低い。従って、このグリースを用いることによって、グリースを施用すべき機 械部分の満足な潤滑を維持するに必要な再施用の回数は、かなり減らしうる。あ る場合には、機械部分が密閉された容器中に入れられているときは、このグリー スは「終身」の潤滑を与えうる。即ち、その機械部分の寿命の間グリースは更新 される必要はない。そのような施用の例としては、自動車のころがり軸受及び滑 り軸受がある。This grease is more prone to oil bleed than other lithium soap containing greases. is low. Therefore, by using this grease, the machine to which the grease should be applied can The number of reapplications required to maintain satisfactory lubrication of mechanical parts can be significantly reduced. a If the machine parts are placed in a closed container, this grease can provide ``lifetime'' lubrication. That is, the grease is renewed during the life of the mechanical part. There is no need to be done. Examples of such applications include rolling bearings and sliding bearings in automobiles. There is a bearing.

グリース中に存在するリチウム石ケンコンプレックスの量は、組成物金属量基準 にして、好ましくは２〜３０重量％、好ましくは５〜２０重量％である。前記リ チウムコンブレンクス石ケンはＣＩＺ〜ＣＺ４のヒドロキシ脂肪酸のリチウム石 ケン及び少なくとも１種の他のリチウム化合物を含むのが好ましい。この他のリ チウム化合物は、有利には、０２〜ＣＩ２の脂肪族ジカルボン酸のリチウム石ケ ンもしくはホウ酸のリチウム塩、又はこれらの混合物である。The amount of lithium soap complex present in the grease is based on the amount of metal in the composition. The amount is preferably 2 to 30% by weight, preferably 5 to 20% by weight. The above Thiium complex stone is a lithium stone of hydroxy fatty acids of CIZ to CZ4. Preferably it contains Ken and at least one other lithium compound. This other link The lithium compound is advantageously a lithium salt of an aliphatic dicarboxylic acid from 02 to CI2. or a lithium salt of boric acid, or a mixture thereof.

より好ましくは、前記ヒドロキシ脂肪酸のリチウム石ケンはＣＩ６〜Ｃ２゜のヒ ドロキシ脂肪酸である。特に好ましいヒドロキシ脂肪酸は、ヒドロキシステアリ ン酸、例えば９−ヒドロキシ−１１０−ヒドロキシ−１又は１２−ヒドロキシス テアリン酸、更に好ましくは後者、である。１２−ヒドロキシステアリン酸の不 飽和形で、二重結合を９−１０位に有するリシノール酸も用いうる。他の適当な ヒドロキシ脂肪酸としては、１２−ヒドロキシベヘン酸及び１ｏ−ヒドロキシバ ルミチン酸がある。More preferably, the hydroxy fatty acid lithium soap has a CI6 to C2°. It is a droxy fatty acid. Particularly preferred hydroxy fatty acids are hydroxy stearyl acids such as 9-hydroxy-110-hydroxy-1 or 12-hydroxys Tearic acid, more preferably the latter. 12-Hydroxystearic acid Ricinoleic acid in saturated form and having a double bond in the 9-10 positions may also be used. other suitable Hydroxy fatty acids include 12-hydroxybehenic acid and 1o-hydroxybutyric acid. Contains lumitic acid.

他のリチウム含有化合物が脂肪族ジカルボン酸である場合は、用いられるヒドロ キシ脂肪酸に対するジカルボン酸の比は、重量比にして、ヒドロキシ脂肪酸１部 あたり、−ａに、０．０５部と１部の間、通常、０．１部と０．８部の間である 。前記ジカルボン酸は、好ましくは０４〜ＣＩ２の、より好ましくはＣ１〜Ｃ１ ゜の脂肪族ジカルボン酸である。適当な酸の例としては、蓚酸、マロン酸、コハ ク酸、グルタル酸、アジピン酸、スペリン酸、ピメリン酸、アゼライン酸、ドデ カンジオン酸（ｄｏｄｅｃａｎｅｄｉｏｎｉｃａｃｉｄ）及びセバシン酸がある 。アゼライン酸及びセバシン酸が特に好ましい。If the other lithium-containing compound is an aliphatic dicarboxylic acid, the hydrocarbon used The ratio of dicarboxylic acid to hydroxy fatty acid is 1 part by weight of hydroxy fatty acid. per -a, between 0.05 and 1 part, usually between 0.1 and 0.8 parts . The dicarboxylic acid is preferably from 04 to CI2, more preferably from C1 to C1. It is an aliphatic dicarboxylic acid of °. Examples of suitable acids include oxalic acid, malonic acid, and oxalic acid. Citric acid, glutaric acid, adipic acid, speric acid, pimelic acid, azelaic acid, dode Candionic acid (dodecanedionic acid) and sebacic acid . Azelaic acid and sebacic acid are particularly preferred.

他のリチウム含有化合物がホウ酸のリチウム塩であるときは、用いられるホウ酸 に対するヒドロキシ脂肪酸の割合は、−ｔＣに、重量比にして、ホウ酸１部に対 してヒドロキシ脂肪酸３〜１００部、通常５〜８０部である。When the other lithium-containing compound is a lithium salt of boric acid, the boric acid used The ratio of hydroxy fatty acid to 1 part of boric acid is -tC in terms of weight ratio. The amount of hydroxy fatty acid is 3 to 100 parts, usually 5 to 80 parts.

このリチウム石ケンコンプレックスは、第２のヒドロキシカルボン酸をも含みう る。これは、一般に炭素原子数３〜１４であり、カルボキシル基から離れること ６炭素以下の原子に付いた一〇Ｈ基を有する。この酸は、例えば乳酸、６−ヒド ロキシデカン酸、３−ヒドロキシ酪酸、１−ヒドロキシカプロン酸、４−ヒドロ キシ酪酸、６−ヒドロキシ−α−ヒドロキシステアリン酸等、又は芳香族酸、例 エバｐ−１＝Ｆｏ−ｔ−シー安息香酸、サリチル酸、２−ヒドロキシ−４−ヘキ シル安、き香酸、ｍ−ヒドロキシ安息香酸、２，５−ジヒドロキシ安息香酸（ゲ ンチシン酸）、２．６−ジヒドロキシ安息香酸（Ｔ−レゾルノン酸）、４−ヒド ロキシ−４−メトキシ安息香酸等、又はヒドロキシ芳香族脂肪族酸、例えば。− ヒドロキシフェニル酢酸、ｍ−ヒドロキシフェニル酢酸、もしくは、ｐ−ヒドロ キシフェニル酢酸である。脂環式ヒドロキシ酸、例えばヒドロキシシクロペンチ ルカルボン酸又はヒドロキシナフテン酸も用いえよう。特に有用なヒドロキシ酸 は、乳酸、サリチル酸及びｐ−ヒドロキシ安息香酸である。This lithium soap complex may also contain a second hydroxycarboxylic acid. Ru. It generally has 3 to 14 carbon atoms and is separated from the carboxyl group. It has an 10H group attached to an atom of up to 6 carbons. This acid is, for example, lactic acid, 6-hydroxy Roxydecanoic acid, 3-hydroxybutyric acid, 1-hydroxycaproic acid, 4-hydro xybutyric acid, 6-hydroxy-α-hydroxystearic acid, etc., or aromatic acids, e.g. Eva p-1 = Fo-t-benzoic acid, salicylic acid, 2-hydroxy-4-hex Sylbenzoic acid, m-hydroxybenzoic acid, 2,5-dihydroxybenzoic acid antisic acid), 2,6-dihydroxybenzoic acid (T-resornoic acid), 4-hydro Roxy-4-methoxybenzoic acid, etc., or hydroxyaromatic aliphatic acids, e.g. − Hydroxyphenylacetic acid, m-hydroxyphenylacetic acid, or p-hydro It is xyphenylacetic acid. Alicyclic hydroxy acids, e.g. hydroxycyclopentyl Carboxylic acids or hydroxynaphthenic acids could also be used. Especially useful hydroxy acids are lactic acid, salicylic acid and p-hydroxybenzoic acid.

これらフリーの酸に代えて、上記第２のヒドロキシカルボン酸の低級アルキルエ ステル、通常はＣ，〜Ｃ４エステルを用いうる。不溶性塩のエステル助剤分散液 としてホウ酸が用いられるときは、これは特に有利である。好ましいエステルの 例として、サリチル酸メチルがある。グリース組成物中に第２のヒドロキシカル ボン酸が用いられるときは、その割合は、重量比にして、前記他のリチウム含有 化合物の酸成分、例えばホウＭ１部あたり、第２ヒドロキシカルボン酸が一般に ０．１〜１０部、通常は０．５〜５部である。In place of these free acids, the lower alkyl ether of the second hydroxycarboxylic acid is used. A ester, usually a C, to C4 ester, may be used. Ester auxiliary dispersion of insoluble salts This is particularly advantageous when boric acid is used as the acetic acid. preferred ester An example is methyl salicylate. A second hydroxyl in the grease composition When a bonic acid is used, its proportion, by weight, is higher than the other lithium-containing acid. Per part of the acid component of the compound, e.g. The amount is 0.1 to 10 parts, usually 0.5 to 5 parts.

前記有機金属化合物の金属は、好ましくは、モリブデンである。The metal of the organometallic compound is preferably molybdenum.

この化合物の有機成分は、好ましくは、チオカルバメート又はキサンテートであ る。従って好ましい有機金属化合物はチオカルバミン酸モリブデン化合物類及び キサントゲン酸モリブデン化合物類である。ジアルキルジチオカルバミン酸モリ ブデン及びジアルキルジチオカルバミン酸モリブデン酸化硫化物（ｏｘｙｓｕｌ ｆ　１ｄｅ）。The organic component of this compound is preferably a thiocarbamate or a xanthate. Ru. Therefore, preferred organometallic compounds are molybdenum thiocarbamate compounds and Molybdenum xanthate compounds. Mori dialkyldithiocarbamate Budene and dialkyldithiocarbamate molybdenum oxysulfide (oxysulfide) f　1de).

グリース組成物中に存在する有機金属化合物の好ましい量は、組成物の全型Ｉ基 準で０．１〜１０重量％であり、より好ましくは０．５〜５重量％である。この 有機金属化合物は耐摩耗性添加剤として働き、グリースの高温寿命を長くする。The preferred amount of organometallic compound present in the grease composition includes all Type I groups in the composition. The amount is generally 0.1 to 10% by weight, more preferably 0.5 to 5% by weight. this Organometallic compounds act as antiwear additives and extend the high temperature life of the grease.

好ましい態様においては、本発明のグリースは、酸化防止剤も含んでし・でもよ （、これは組成物全重量を基準にして０．１〜５重量％、好ましくは０．５〜３ 重量％で存在する。用いられる酸化防止剤は、好ましくは、アミンベースの酸化 防止剤化合物で、例えばアルキルジフェニルアミンである。In a preferred embodiment, the grease of the invention may also contain an antioxidant. (, this is 0.1 to 5% by weight, preferably 0.5 to 3% by weight, based on the total weight of the composition) Present in % by weight. The antioxidant used is preferably an amine-based oxidant. Inhibitor compounds, such as alkyldiphenylamines.

このグリース組成物に用いられる潤滑用基油は、一般に用いられている潤滑油の 基油のいずれでもよく、好ましくは、鉱油又は鉱油と合成油の配合物である。一 般にこれらの潤滑油は２１０°Ｆで３５〜３００ＳＵＳの範囲内の成る粘度、及 び３０〜１７０、好ましくは、３０〜１４０の範囲内の成る粘度指数を持つ、こ のグリースを調製するのに用いられる鉱物性潤滑油ベースストック（ｂａｓｅｓ ｔｏｃｋ）としては、パラフィン性基原油（ｂａｓｅ　ｃｒｕｄｅ）、ナフテン 性基原油及び混合基原油から誘導される一般的に精製されたベースストックのい ずれであってもよい、用いうる合成潤滑用油としては、二塩基酸のエステル、例 えばセパシン酸ジー２−エチルヘキシル、グリコールのエステル例えばテトラエ チレングリコールのＣＩ！オキソ酸ジエステル、又は複合エステル、例えば１モ ルのセバシン酸及び２モルのテトラエチレングリコール及び２モルの２−エチル ヘキサン酸から形成されるものが例示できる。用いうる他の合成油としては、合 成炭化水素、例えばアルキルベンゼン、例えばベンゼンをテトラプロピレンでア ルキル化して得られるアルキレートボトム（ｂｏｔｔｏｍ）、又はα−オレフィ ンのポリマー又はコポリマー；シリコーン油、例えばエチルフェニルポリシロキ サン、メチルポリシロキサン等；ポリグリコールオイル、例えばブチルアルコー ルをプロピレンオキサイドで縮合して得られるもの一カーボネートエステル、例 えばＣ８オキソアルコールをエチルカーボネートと反応させて半エステルを形成 した後この半エステルをテトラエチレングリコールと反応させて得られる製品等 を含む、他の適当な合成油としては、ポリフェニルエーテル、例えば約３〜７エ ーテル結合及び約４〜８のフェニル基を有するもの（米国特許患３．４２４，６ ７８　、カラム３を参照のこと）がある。The lubricating base oil used in this grease composition is one of the commonly used lubricating oils. Any base oil may be used, preferably mineral oil or a blend of mineral oil and synthetic oil. one Generally, these lubricants have viscosities in the range of 35 to 300 SUS at 210°F, and and a viscosity index in the range of 30 to 170, preferably 30 to 140. Mineral lubricating oil base stocks used to prepare greases (tock), paraffinic base crude oil, naphthene Commonly refined base stocks derived from base crude oils and mixed base crude oils. Synthetic lubricating oils that may be used include esters of dibasic acids, e.g. For example di-2-ethylhexyl sepacate, esters of glycols such as tetraethylhexyl CI of tyrene glycol! Oxoacid diester or complex ester, e.g. 1 mole of sebacic acid and 2 moles of tetraethylene glycol and 2 moles of 2-ethyl An example is one formed from hexanoic acid. Other synthetic oils that can be used include Aqueous hydrocarbons such as alkylbenzenes such as benzene with tetrapropylene alkylate bottom obtained by alkylation, or α-olefin polymers or copolymers of silicone oils, such as ethyl phenyl polysiloxane; San, methylpolysiloxane, etc.; polyglycol oil, e.g. butyl alcohol Carbonate esters obtained by condensation of 1 with propylene oxide, e.g. For example, reacting a C8 oxo alcohol with ethyl carbonate to form a half ester After that, products obtained by reacting this half ester with tetraethylene glycol, etc. Other suitable synthetic oils include polyphenyl ethers, e.g. ter bond and about 4 to 8 phenyl groups (U.S. Pat. No. 3,424,6 78, see column 3).

本発明のグリースは、高温での寿命が長いという利点に加えてリチウムコンプレ ックスグリースに付随する通常の利点も保持するという長所をも持つ。In addition to the advantage of long life at high temperatures, the grease of the present invention is lithium-component. It also has the advantage of retaining the usual benefits associated with grease.

以下の例によって本発明を説明する。これらの例の全グリースは、ＮＬＧ　ｒグ レード２のコンシスチンシーとなるように作った。即ち、全グリースは、ＡＳＴ Ｍ法Ｄ２１７又はＤ２６６５で測定して、２５°Ｃでの６０往復混和ちょう度が ２６５〜２９５である。The invention is illustrated by the following examples. All greases in these examples are NLG r It was made to have a consistency of Rade 2. That is, all grease is AST Measured with M method D217 or D2665, 60 round work penetration at 25°C It is 265-295.

例１〜４ 例１〜３は、ヒドロキシ脂肪酸のリチウム石ケン及び脂肪族ビスカルボン酸のリ チウム石ケンを含むリチウムコンプレックスをへ一スにした本発明のグリース組 成物を例示する。例４は、同しリチウム石ケンコンプレックスを用いる比較例で ある。Examples 1-4 Examples 1 to 3 are lithium soaps of hydroxy fatty acids and lithium soaps of aliphatic biscarboxylic acids. Grease set of the present invention containing a lithium complex containing lithium soap Examples of products are shown below. Example 4 is a comparative example using the same lithium stone complex. be.

例１〜４の試験結果は表１にまとめて示す。The test results of Examples 1 to 4 are summarized in Table 1.

例１ リチウムコンプレックスグリースを、次の成分と配合した：底−−兄　！工Ｘ パラフィン基油　８０．５ （Ｖａｏ＝１５０ｍ”　／ｓ、ＶＩ＝９１）’水酸化リチウムー水塩　２．５ １２−ヒドロキシステアリンａ　１１．０アゼライン酸　２．０ ジアルキルジチオカルバミン酸 モリブデン酸化硫化物２２．５ アルキルジフェニルアミン３１．５ （１）　■、、＝　４ｏ°Ｃでの粘度、ｖＩ　＝粘度指数（２）アサヒ電化工業 （株）から５ａｋｕｒａｌｕｂｅ　６００として供給された。Example 1 Lithium complex grease is blended with the following ingredients: Bottom--Brother! Engineering Paraffin base oil 80.5 (Vao=150m”/s, VI=91)’Lithium hydroxide-water salt 2.5 12-Hydroxystearin a 11.0 Azelaic acid 2.0 dialkyldithiocarbamic acid Molybdenum oxidized sulfide 22.5 Alkyldiphenylamine 31.5 (1) ■,, = viscosity at 4o°C, vI = viscosity index (2) Asahi Denka Kogyo It was supplied as 5akuralube 600 by Co., Ltd.

（３）チバーガイギー社からＩｒｇａｎｏｘ　Ｌ５７として供給された。(3) Supplied as Irganox L57 from Civer-Geigy.

前記基油成分及びリチウム石ケンコンプレックス成分は英国特許Ｎ１１１，３８ ４，９０４の例１に述べられたようにして配合した０次いでこのグリースにジア ルキルジチオカルバミン酸モリブデン酸化硫化物（ｇｏｌｙｂｕｄｅｎｕｓ＋　 ｏｘｙｓｕｌｐｈｉｄｅ　ｄｉａｌｋｙｌｄｉｔｈｉｏｃａｒｂａｍａｔｅ）　 （Ｍ　Ｄ　Ｄ　Ｃ）及びアルキルジフェニルアミン添加剤を加え、このグリース を通常のグリースミルを用いて粉砕した。The base oil component and the lithium soap complex component are disclosed in British Patent N111,38. This grease was then formulated as described in Example 1 of 4,904. molybdenum oxidized sulfide rukyldithiocarbamate (golybudenus+) oxysulfide dialkyldithiocarbamate) (M　D　DC　C) and an alkyldiphenylamine additive, was ground using a regular grease mill.

このグリースの高温での寿命は、標準試験ＤＩＮ　５１８２１Ｔ２Ａ／１５００ ／６０００に従って測定した。この試験においては、５つのベアリングが１セツ トになったものを、特定の温度、荷重及び速度の条件の下で運転する。潤滑飢餓 のために、必要な駆動運動量が高くなり過ぎると、同期発電機は、自動的に運転 停止する。The life of this grease at high temperatures is determined by standard test DIN 51821T2A/1500. /6000. In this test, five bearings were assembled in one set. The machine is then operated under specified temperature, load and speed conditions. lubrication starvation If the required drive momentum becomes too high due to Stop.

こうして５つの潤滑油の寿命が得られ、次のデータが計算される二Ｆ１゜；これ は、その後にヘアリングの最初の１０％が潤滑飢餓を起こす時間を表わす。The lives of the five lubricating oils are thus obtained, and the following data are calculated: represents the time after which the first 10% of the hair ring undergoes lubrication starvation.

Ｆ、。：これは、その後にベアリングの５０％が潤滑飢餓を起こす時間を表わす 。F. : This represents the time after which 50% of the bearing will experience lubrication starvation. .

ある与えられた温度でＦ、。の値が少なくとも１００時間であるグリースは、そ の温度での終身の潤滑剤とみなされる。F at a given temperature. Greases with a value of at least 100 hours It is considered a lifelong lubricant at temperatures of

試験の結果を以下の第１表に示す。The results of the test are shown in Table 1 below.

例２ 用いたＭＤＤＣがＶａｎｄｅｒｂｉｌｔ　Ｃｏｍｐａｎｙ　［ｎｃ、から門ｏ１ ｙｖａｎ　Ａとして供給されたことを除いて、例１と同様にしてグリース組成物 を配合した。Example 2 The MDDC used was from Vanderbilt Company [nc, gate o1 Grease composition as in Example 1 except that it was supplied as yvan A. was blended.

このグリースを例１に述べたのと同様にして試験した。その結果を以下の第１表 に示す。This grease was tested in the same manner as described in Example 1. The results are shown in Table 1 below. Shown below.

例３ アルキルジフェニルアミンを除き、ＭＤＤＣの量を３重量％に増した他は、例１ と同様にしてグリース組成物を配合した。基油の量を８１．５重量％に増すこと によりバランスをとった。Example 3 Example 1 except that the alkyldiphenylamine was removed and the amount of MDDC was increased to 3% by weight. A grease composition was mixed in the same manner as above. Increase the amount of base oil to 81.5% by weight Balanced by.

このグリースを例１に述べたようにして試験した。その結果を以下の第１表に示 す。This grease was tested as described in Example 1. The results are shown in Table 1 below. vinegar.

例４ 例１〜３のグリースを従来のリチウムコンプレックス石ケングリースと比較した 。このグリースは、上記例と同し基油及びリチウムコンプレックスを含んでいた が、モリブデン化合物もアルキルジフェニルアミンも含んでいなかった。Example 4 The greases of Examples 1 to 3 were compared with conventional lithium complex Sekiken grease. . This grease contained the same base oil and lithium complex as in the example above. However, it contained neither molybdenum compounds nor alkyldiphenylamines.

この比較用グリースを例１に述べたようにして試験した。その結果を以下の第１ 表に示す。This comparative grease was tested as described in Example 1. The result is shown in the first section below. Shown in the table.

４　（ｒ）　６６／７２ 本発明のグリース組成物は、同し基油及びリチウムコンプレックスを用いる比較 グリースよりも大巾に長い寿命を持つことを、この結果は示している０例えば、 １４０°Ｃで、グリース１は比較グリース４の５倍以上の寿命を持っている。4 (r) 66/72 The grease composition of the present invention compares favorably with the same base oil and lithium complex. This result shows that it has a much longer lifespan than grease.0For example, At 140°C, Grease 1 has a lifespan more than five times longer than Comparative Grease 4.

例５及びに れらの２つの例は、ヒドロキシ脂肪酸のリチウム石ケン及びホウ酸のリチウム塩 を含むリチウムコンプレックスに基づく本発明のグリースを明示し、かつこのグ リースを、同じリチウム石ケンコンプレックスを含む従来のグリースと比較する 。その結果をまとめて第２表に示す。Example 5 and Two examples of these are lithium soaps of hydroxy fatty acids and lithium salts of boric acid. The grease of the invention is based on a lithium complex containing Compare Lease with conventional greases containing the same lithium soap complex . The results are summarized in Table 2.

例５ 次の成分を用いてグリース組成物を配合した：底−一立　立上Ｘ パラフィン基油　７Ｂ、３ （Ｖａｅ＝　１１０　ｗａ”　／　ｓ、ＶＩ＝９５）’水酸化リチウムー水和物 　３．５ １２−ヒドロキシステアリン酸　１１．０ホウ酸　０．９ サリチル酸メチル　２．３ Ｍ　Ｄ　Ｄ　Ｃ”　２．５ ヱ土上丑ジ１」三」りｊユ已−−−一−−−−−−−−退１（１）Ｖ、。＝４０ °Ｃでの粘度、ＶＩ＝粘度率（２）アサヒ電化工業（株）から５ａｋｕｒａｌｕ ｂｅ　６００として供給された。Example 5 A grease composition was formulated using the following ingredients: Bottom-Ichi-Rise-X Paraffin base oil 7B, 3 (Vae=110 wa"/s, VI=95)'Lithium hydroxide hydrate 3.5 12-Hydroxystearic acid 11.0 Boric acid 0.9 Methyl salicylate 2.3 M　D　D　C”　2.5 1 (1) V. =40 Viscosity at °C, VI = viscosity coefficient (2) 5akuralu from Asahi Denka Kogyo Co., Ltd. Supplied as be600.

（３）チハーガイギー社からＩｒｇａｎｏｘ　Ｌ５７として供給Ｃ及びアルキル ジフェニルアミン添加剤を加え、このグリースを通　−常のグリースミルを用い て粉砕した。(3) C and alkyl supplied as Irganox L57 from Cihar Geigy Add the diphenylamine additive and run this grease through a conventional grease mill. and crushed it.

このグリースを例１に述べられたようにして試験した。その結果を、以下の第２ 表に示す。This grease was tested as described in Example 1. The results are shown in the second section below. Shown in the table.

例６ 比較のためにＭＤＤＣ及びアルキルジフェニルアミンを除いた他は、例５のグリ ースと同しリチウム石ケンコンプレンクスを含む通常のリチウムコンブレンクス グリースを、例１に述べたようにして試験した。その結果を以下の第２表に示す 。Example 6 The glycerin of Example 5 except that MDDC and alkyldiphenylamine were removed for comparison. Ordinary lithium complex containing the same lithium stone complex as base The grease was tested as described in Example 1. The results are shown in Table 2 below. .

第２表 グリース組成物 これらの結果は、１６０°ＣでのＦ＋ｏ寿命は約６０時間で互に匹敵するが、グ リース５、即ち本発明のグリースのＦ、。寿命は、比較グリース６のＦ、。寿命 よりも１．７倍大きい。Table 2 grease composition These results show that the F+o lifetime at 160°C is comparable to each other at about 60 hours, but Grease 5, F of the grease of the invention. The lifespan is F of Comparative Grease 6. lifespan 1.7 times larger than .

例７ 前記パラフィン基油を、全グリース組成物を基準にして２８．５重量％のポリ− α−オレフィン（Ｖ４１１＝　４８　ｍ”　／　ｓ、Ｖ−ｏｏ＝７．９ｍ”／ｓ ）及び全グリース組成物を基準にして５０重量％のパラフィン基油（Ｖ４ａ＝　 １００　Ｍ”　／　Ｓ、Ｖ＋ａｏ　＝　１２ｍ”　／　ｓ　）の基油配合物で置 き換える他は例２と同様にしてグリース組成物を配合した。前記の配合した基油 は次の粘度を示した：ＦＩＧの結果は１０１時間であり、Ｆ、。の結果は１３４ 時間であった。Example 7 The paraffinic base oil was combined with 28.5% by weight of poly-based oil based on the total grease composition. α-olefin (V411=48 m”/s, V-oo=7.9 m”/s ) and 50% by weight based on the total grease composition paraffin base oil (V4a= 100 M”/S, V+ao = 12 m”/s) base oil formulation. A grease composition was formulated in the same manner as in Example 2, except for changing the composition. Base oil blended above showed the following viscosity: FIG result was 101 hours, F. The result is 134 It was time.

従ってこのグリースを高温度で長い寿命を示した。Therefore, this grease exhibited a long service life at high temperatures.

要約書 大部分の割合の潤滑用基油、リチウム石ケンコンプレックス及び存機金属化合物 を含む潤滑用グリース組成物。前記有機金属化合物の金属は、モリブデン、タン グステン、バナジウム、ニオブ及びタンタルから選ばれ、好ましくはモリブデン である。このグリースは減摩ヘアリングのような機械部分を潤滑するために用い ることができ、高温で長寿命を示す。abstract Majority of lubricating base oil, lithium soap complex and existing metal compounds A lubricating grease composition containing. The metal of the organometallic compound is molybdenum, tan selected from gsten, vanadium, niobium and tantalum, preferably molybdenum It is. This grease is used to lubricate mechanical parts such as anti-friction hair rings. It has a long lifespan at high temperatures.

補正書の翻訳文提出書 （特許法第１８４条の８） 平成４年７月　≠日Submission of translation of written amendment (Article 184-8 of the Patent Act) July 1992 ≠ day

Claims (15)

【特許請求の範囲】[Claims] １．大部分の割合の潤滑用基油、増粘量のリチウム石ケンコンプレックス及び有 効量の、金属がモリブデン、タングステン、バナジウム、ニオブ及びタンタルか ら選ばれる有機金属化合物を含む潤滑用グリース組成物。1. Large proportion of lubricating base oil, thickening amount of lithium soap complex and Effective amounts of metals such as molybdenum, tungsten, vanadium, niobium and tantalum A lubricating grease composition containing an organometallic compound selected from ２．前記有機金属化合物の金属がモリブデンである請求の範囲１のグリース組成 物。2. The grease composition according to claim 1, wherein the metal of the organometallic compound is molybdenum. thing. ３．前記有機金属化合物の有機成分がチオカルバメート又はキサンテートである 請求の範囲１又は２のグリース組成物。3. The organic component of the organometallic compound is a thiocarbamate or xanthate. The grease composition according to claim 1 or 2. ４．前記有機金属化合物がジアルキルジチオカルバミン酸モリブデン酸化硫化物 である先行の請求の範囲のいずれかのグリース組成物。4. The organometallic compound is dialkyldithiocarbamate molybdenum oxysulfide The grease composition of any of the preceding claims. ５．前記組成物中に存在する有機金属化合物の量がこの組成物全量量を基準にし て０．１〜１０重量％である先行の請求の範囲のいずれかのグリース組成物。5. The amount of organometallic compound present in the composition is based on the total amount of the composition. Grease composition according to any of the preceding claims, wherein the grease composition is from 0.1 to 10% by weight. ６．前記リチウム石ケンがＣ１２〜Ｃ２４のヒドロキシ脂肪酸のリチウム石ケン 及び少なくとも１つの他のリチウム含有化合物を含む先行の請求の範囲のいずれ かのグリース組成物。6. The lithium soap is a C12-C24 hydroxy fatty acid lithium soap. and at least one other lithium-containing compound. Grease composition. ７．前記他のリチウム含有化合物がＣ２〜Ｃ１２の脂肪族ジカルボン酸のリチウ ム石ケンである請求の範囲６のグリース組成物。7. The other lithium-containing compound is lithium of a C2 to C12 aliphatic dicarboxylic acid. The grease composition according to claim 6, which is a mineral oil. ８．前記他のリチウム含有化合物がホウ酸のリチウム塩である請求の範囲６のグ リース組成物。8. The group according to claim 6, wherein the other lithium-containing compound is a lithium salt of boric acid. wreath composition. ９．前記リチウム石ケンコンプレックスが、カルボキシル基から離れること６炭 素以下に−ＯＨ基を有するＣ３〜Ｃ１４のヒドロキシカルボン酸のリチウム石ケ ンも含む請求の範囲６〜８のいずれかのグリース組成物。9. The lithium soap complex separates from the carboxyl group. Lithium salt of C3-C14 hydroxycarboxylic acid having -OH group below 9. The grease composition according to any one of claims 6 to 8, further comprising: １０．前記組成物中に存在するリチウム石ケンコンプレックスの量が、組成物の 全量量を基準にして２〜３０重量％である先行の請求の範囲のいずれかに記載の グリース組成物。10. The amount of lithium soap complex present in the composition 2 to 30% by weight based on the total amount according to any of the preceding claims. Grease composition. １１．酸化防止剤も含む先行の請求の範囲のいずれかのグリース組成物。11. The grease composition of any of the preceding claims also comprising an antioxidant. １２．前記酸化防止剤がアルキルジフェニルアミンである請求の範囲１１のグリ ース組成物。12. The glycerol according to claim 11, wherein the antioxidant is an alkyldiphenylamine. composition. １３．前記組成物中に存在する酸化防止剤の量が、組成物全重量を基準にして０ ．１〜５重量％である請求の範囲１１又は１２のグリース組成物。13. The amount of antioxidant present in the composition is 0 based on the total weight of the composition. ．． The grease composition according to claim 11 or 12, wherein the content is 1 to 5% by weight. １４．前記基油が鉱油又は鉱油と合成油との混合物である先行の請求の範囲のい ずれかのグリース組成物。14. In any of the preceding claims, the base oil is mineral oil or a mixture of mineral oil and synthetic oil. Any grease composition. １５．例１〜３，５又は７のいずれかに実質的に記載した潤滑用グリース組成物 。15. Lubricating grease composition substantially as described in any of Examples 1-3, 5 or 7 .
JP3504602A 1990-03-07 1991-03-05 Lubricating grease composition Expired - Fee Related JP2964165B2 (en)

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JPH093468A (en) * 1995-04-21 1997-01-07 Hitachi Ltd Lubricating oil composition and lubricating grease composition
JP2001187891A (en) * 1995-04-21 2001-07-10 Hitachi Ltd Lubricating oil composition and lubricating grease composition
JP2001335792A (en) * 2000-03-21 2001-12-04 Nsk Ltd Lubricating grease composition, and roller bearing and rolling device using this composition

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GB9223945D0 (en) * 1992-11-14 1993-01-06 Gkn Technology Ltd Greases
JP3608805B2 (en) * 1993-04-30 2005-01-12 東燃ゼネラル石油株式会社 Lubricating oil composition
CA2171537A1 (en) * 1993-09-13 1995-03-23 Harold Shaub Mixed antioxidant composition
US6482779B2 (en) 2000-03-21 2002-11-19 Nsk Ltd. Lubricating grease composition and rolling apparatus comprising same
CN101200670B (en) * 2006-12-12 2010-05-19 中国石油天然气集团公司 Composite lithium-base grease and method for making same
CN101880581A (en) * 2010-06-29 2010-11-10 濮阳市航天化工有限公司 Universal lithium base grease and preparation method thereof
CN101880582A (en) * 2010-06-29 2010-11-10 濮阳市航天化工有限公司 High-temperature grease and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH093468A (en) * 1995-04-21 1997-01-07 Hitachi Ltd Lubricating oil composition and lubricating grease composition
JP2001187891A (en) * 1995-04-21 2001-07-10 Hitachi Ltd Lubricating oil composition and lubricating grease composition
JP2001335792A (en) * 2000-03-21 2001-12-04 Nsk Ltd Lubricating grease composition, and roller bearing and rolling device using this composition

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EP0523064A1 (en) 1993-01-20
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