EP0765374B1 - Schmierfettzusammensetzung - Google Patents

Schmierfettzusammensetzung Download PDF

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Publication number
EP0765374B1
EP0765374B1 EP95923825A EP95923825A EP0765374B1 EP 0765374 B1 EP0765374 B1 EP 0765374B1 EP 95923825 A EP95923825 A EP 95923825A EP 95923825 A EP95923825 A EP 95923825A EP 0765374 B1 EP0765374 B1 EP 0765374B1
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EP
European Patent Office
Prior art keywords
grease
acid
polyalkenyl
grease composition
lithium
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.)
Expired - Lifetime
Application number
EP95923825A
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English (en)
French (fr)
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EP0765374A1 (de
Inventor
Hiromitsu Ikeuchi
Takeo Kobayashi
Shin Shigano
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.)
ExxonMobil Technology and Engineering Co
Original Assignee
ExxonMobil Research and Engineering Co
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Publication of EP0765374A1 publication Critical patent/EP0765374A1/de
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    • 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
    • C10M169/06—Mixtures of thickeners and additives
    • 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
    • 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
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    • 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
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/30—Lubricating compositions characterised by the thickener being a macromolecular compound containing atoms of elements not provided for in groups C10M119/02 - C10M119/28
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/86—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of 30 or more atoms
    • C10M129/92—Carboxylic acids
    • C10M129/93—Carboxylic acids having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M129/86—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of 30 or more atoms
    • C10M129/95—Esters
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
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    • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
    • C10M2207/1225—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic used as thickening agent
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    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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    • C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
    • C10M2207/1245—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof used as thickening agent
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    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
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    • C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
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    • C10M2207/1415—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic used as thickening agent
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    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11

Definitions

  • This invention relates to grease compositions having low noise properties and high dropping points.
  • the bearings in modern automobiles and electric appliances are typically sealed bearings.
  • Greases for sealed bearings must provide lubrication for the life of the bearing which places high demands on greases used in such service.
  • Sealed bearing greases must meet numerous performance requirements including extending bearing life, high temperature performance, high dropping point, low oil separation, oxidation stability, fretting wear protection and low noise.
  • lithium complex soap based greases have been used in sealed bearing applications. Such greases offer long service at high temperatures but suffer from generally higher noise than simple lithium soap based greases.
  • This invention relates to a grease composition having improved low noise properties and a dropping point of greater than 270°C according to standard test ASTM D566, which composition comprises:
  • the greases according to the invention provide long bearing life and high dropping point while providing low bearing noise.
  • the lubricating oil base can be any of the conventionally used mineral oils, synthetic hydrocarbon oils or synthetic ester oils, or mixtures thereof depending upon the particular grease being prepared. In general these lubricating oils will have a viscosity in the range of about 5 to about 400 cSt at 40°C, although typical applications will require an oil having a viscosity ranging from about 10 to about 200 cSt at 40°C.
  • Mineral lubricating oil base stocks used in preparing the greases can be any conventionally refined base stocks derived from paraffinic, naphthenic and mixed base crudes.
  • Synthetic lubricating oils that can be used include esters of glycols such as a C 13 oxo acid diester of tetraethylene glycol, or complex esters such as one formed from 1 mole of sebacic acid and 2 moles of tetraethylene glycol and 2 moles of 2-ethylhexanoic acid.
  • synthetic oils that can be used include synthetic hydrocarbons such as polyalphaolefins; alkyl benzenes, e.g., alkylate bottoms from the alkylation of benzene with tetrapropylene, or the copolymers of ethylene and propylene; silicone oils, e.g., ethyl phenyl polysiloxanes, methyl polysiloxanes, etc.; polyglycol oils, e.g., those obtained by condensing butyl alcohol with propylene oxide; carbonate esters, e.g., the product of reacting C 8 oxo alcohol with ethyl carbonate to form a half ester followed by reaction of the latter with tetraethylene glycol, etc.
  • synthetic hydrocarbons such as polyalphaolefins
  • alkyl benzenes e.g., alkylate bottoms from the alkylation of benzene with tetrapropylene, or the
  • Suitable synthetic oils include the polyphenyl ethers, e.g., those having from about 3 to 7 ether linkages and about 4 to 8 phenyl groups.
  • the amount of lubricating oil in the grease can also vary broadly, but, typically, will range from about 50 wt% to about 98 wt%, preferably from about 75 wt% to about 95 wt%, of the grease.
  • the grease composition contains a thickener dispersed in the lubricating base oil to form a grease.
  • Preferred thickeners are lithium soap complex thickeners containing a lithium soap of a C 12 to C 24 hydroxy fatty acid and a second lithium salt compound which is a lithium salt of a C 2 to C 12 aliphatic or cycloaliphatic dicarboxylic acid, a lithium salt of a C 3 to C 14 hydroxy carboxylic acid which has the hydroxy group separated from the carboxyl group by six or less carbon atoms or a mixture thereof.
  • the lithium salt of boric acid may be added as a third thickener component.
  • Preferred hydroxy fatty acids include hydroxystearic, hydroxyricinoleic, hydroxybehenic and hydroxypalmitic. Especially preferred is 12-hydroxystearic acid.
  • the second lithium salt compound is preferably a C 6 to C 10 aliphatic dicarboxylic acid, more preferably azelaic or sebacic acids, especially azelaic acid.
  • the hydroxy-carboxylic acid is preferably lactic acid, salicylic acid or other hydroxy-benzoic acids, more preferably salicylic acid.
  • the amount of lithium soap complex thickeners is preferably from 5 to 20 wt%, based on grease.
  • the ratio of hydroxy fatty acid to aliphatic dicarboxylic acid and/or hydroxy-carboxylic acid is from 10:0.5 to 10:15, preferably 10:1.5 to 10:6.
  • the grease composition will also contain a polyalkenyl succinic anhydride, a polyalkenyl succinic acid or mixture thereof as dispersant.
  • the polyalkenyl group will have a number average molecular weight of from 300 to 4,000, preferably 400 to 2,500.
  • Preferred polyalkenyl groups are poly-C 3 and poly-C 4 olefins, especially polyisobutylene.
  • Polyisobutylene succinic anhydride and/or acid will hereinafter be collectively referred to as PIBSA.
  • the amount of dispersant is preferably from 0.1 wt% to 5 wt%, based on grease.
  • Lithium complex soap greases are prepared by heating hydroxy fatty acid and base oil, adding a concentrated aqueous solution of lithium hydroxide. Heating is continued at elevated temperature to remove most of the water. The reaction mixture is then cooled to about 100°C and dicarboxylic acid is added followed by a second portion of concentrated lithium hydroxide. This mixture is again heated to elevated temperature to again remove water. After heating is completed, the grease mixture is cooled, remaining oil and any other additives added and the grease is worked up using conventional techniques. The preparation may also be accomplished in a single step process by heating, base oil, fatty acid and dicarboxylic acid, then adding lithium hydroxide solution followed by dehydration and adding remaining oil.
  • the grease composition may contain small amounts of supplemental additives which include, but are not limited to, anti-corrosive agents, extreme pressure antiwear agents, pour point depressants, tackiness agents, oxidation inhibitors, dyes and the like, which are incorporated for specific purposes.
  • supplemental additives include, but are not limited to, anti-corrosive agents, extreme pressure antiwear agents, pour point depressants, tackiness agents, oxidation inhibitors, dyes and the like, which are incorporated for specific purposes.
  • the total amount of these additives will typically range from about 2 wt% to about 10 wt% based on total weight of the grease composition.
  • This example illustrates the preparation of a low noise grease.
  • a laboratory kettle was charged with 700 g of refined paraffinic base oil having a viscosity of 90 cSt at 40°C, 139.2 g of 12-hydroxystearic acid, 69.5 g of azelaic and 12.0 g of PIBSA having a polyisobutenyl radical of number average molecular weight of 950.
  • the resulting mixture was heated with stirring until the temperature reached 90°C. At this point, heating was stopped and 345 g of a 15% solution of lithium hydroxide (heated to 90°C) was added with stirring. When addition of the lithium hydroxide solution was complete, heating was resumed to remove water.
  • Grease noise was measured according to the following procedure which is more fully described in Japanese Patent 53-2357. Solid particles in grease result in vibrations which can be converted into an electrical signal. After correcting for race noise of bearings under standard conditions, the electrical signal due to solid particles including soap particles in grease can be measured according to the following procedure.
  • a vibration detection device is attached to the outer ring of the bearings. The detection device converts the vibrations into an electrical signal which is amplified and sent to a zone wave filter.
  • the zone wave filter compares the amplified signal received from the bearings with the known vibration frequency from the bearings alone, filters out the vibration frequencies from the bearings and sends the filtered electronic signal through an amplifier to a clipper circuit.
  • the clipper circuit "clips" the electrical signal from the amplifier at a given level. This level is set so as to measure only peak voltages which correspond to solid particle noise from particles in the grease.
  • the clipping level is set at a value greater than the peak value corresponding to the race noise from the bearings.
  • This example compares the noise properties and dropping point of a grease formulated with a polyisobutenyl succinic anhydride/acid dispersant according to the invention with polyisobutenyl succinic imide type dispersants described in Japanese Patent A2 58125794.
  • Greases were formulated using the procedures of Example 1. Noise was tested using the procedure of Example 2 and dropping point was measured according to test method ASTM D566. The results are set forth in Table 1.
  • Greases formulated with a polyisobutenyl succinic anhydride/ acid type dispersant showed significantly better noise property and higher dropping point compared to a lithium complex grease formulated without dispersant (Sample 4). Samples 1-3 also demonstrated consistently higher dropping points compared to greases formulated with polyisobutenyl succinic imide type dispersants (Comparative Samples 5-13). A commercial lithium complex grease (Sample 14) demonstrated a much inferior noise property compared to Samples 1-3 according to this invention.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Claims (8)

  1. Schmierfettzusammensetzung mit verbesserten Lärmverminderungseigenschaften und einem Tropfpunkt von mehr als 270°C gemäß dem Standardtest ASTM D566, wobei die Zusammensetzung
    a) eine größere Menge eines Schmierbasisöls,
    b) 2 bis 30 Gew.%. bezogen auf die Schmierfettzusammensetzung, von einem Lithiumseifenkomplex-Verdickungsmittel und
    c) 0,1 bis 10 Gew.%, bezogen auf die Schmierfettzusammensetzung, von einem Polyalkenylbernsteinsäureanhydrid, einer Polyalkenylbernsteinsäure oder einer Mischung davon, wobei die Polyalkenylgruppe ein durchschnittliches Molekulargewicht (Zahlenmittel) von 300 bis 4000 hat,
    enthält.
  2. Schmierfettzusammensetzung nach Anspruch 1, bei der das Lithiumseifenkomplex-Verdickungsmittel eine Lithiumseife einer C12- bis C24-Hydroxyfettsäure und ein Lithiumsalz einer aliphatischen oder cycloaliphatischen C2- bis C12- Dicarbonsäure, ein Lithiumsalz einer C3- bis C14-Hydroxycarbonsäure oder eine Mischung davon enthält.
  3. Schmierfettzusammensetzung nach Anspruch 2, bei der das Lithiumseifenkomplex-Verdickungsmittel eine Lithiumseife von 12-Hydroxystearinsäure und ein Lithiumsalz von Azelainsäure und/oder Lithiumsalz von Salicylsäure enthält.
  4. Schmierfettzusammensetzung nach Anspruch 2 oder 3, bei der das Verhältnis von Hydroxyfettsäure zu aliphatischer oder cycloaliphatischer Dicarbonsäure und/oder Hydroxycarbonsäure 10:0,5 bis 10:15 beträgt.
  5. Schmierfettzusammensetzung nach einem der vorhergehenden Ansprüche, bei der die Polyalkenyleinheit in dem Polyisobutenylbernsteinsäureanhydrid und/oder der Polyisobutenylbernsteinsäure ein durchschnittliches Molekulargewicht (Zahlenmittel) von 400 bis 2500 hat.
  6. Verfahren zur Verbesserung der Lärmverminderung und zur Lieferung eines Tropfpunkts von mehr als 270°C (ASTM D566) bei einem Schmierfett, bei dem in ein Basisöl 2 bis 30 Gew.%, bezogen auf das Schmierfett, von einem Lithiumseifenkomplex-Verdickungsmittel und 0,1 bis 10 Gew.%, bezogen auf das Schmierfett, von einem Polyisobutenylbernsteinsäureanhydrid, einer Polyisobutenylbernsteinsäure oder einer Mischung davon eingebracht wird, wobei die Polyalkenylgruppe ein durchschnittliches Molekulargewicht (Zahlenmittel) von 300 bis 4000 hat.
  7. Verwendung von einem Polyalkenylbernsteinsäureanhydrid, einer Polyalkenylbernsteinsäure oder einer Mischung davon, wobei die Polyalkenylgruppe ein durchschnittliches Molekulargewicht (Zahlenmittel) von 300 bis 4000 hat, in einer Menge von 0,1 bis 10 Gew.%, bezogen auf das Schmierfett, in einer Schmierfettzusammensetzung, die 2 bis 30 Gew.%, bezogen auf das Schmierfett, eines Lithiumseifenkomplex-Verdikkungsmittels enthält, zur Verbesserung der Lärmverminderungseigenschaften der Schmierfettzusammensetzung.
  8. Verwendung von einem Polyalkenylbernsteinsäureanhydrid, einer Polyalkenylbernsteinsäure oder einer Mischung davon, wobei die Polyalkenylgruppe ein durchschnittliches Molekulargewicht (Zahlenmittel) von 300 bis 4000 hat, in einer Menge von 0,1 bis 10 Gew.%, bezogen auf das Schmierfett, in einer Schmierfettzusammensetzung, die 2 bis 30 Gew.%, bezogen auf das Schmierfett, eines Lithiumseifenkomplex-Verdikkungsmittels enthält, zur Verbesserung des Tropfpunkts der Schmierfettzusammensetzung.
EP95923825A 1994-06-17 1995-06-12 Schmierfettzusammensetzung Expired - Lifetime EP0765374B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US26149194A 1994-06-17 1994-06-17
US261491 1994-06-17
PCT/US1995/007471 WO1995035355A1 (en) 1994-06-17 1995-06-12 Grease composition

Publications (2)

Publication Number Publication Date
EP0765374A1 EP0765374A1 (de) 1997-04-02
EP0765374B1 true EP0765374B1 (de) 2001-12-05

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EP (1) EP0765374B1 (de)
JP (1) JP3762432B2 (de)
CA (1) CA2191481C (de)
DE (1) DE69524412T2 (de)
WO (1) WO1995035355A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE112006003061T5 (de) 2005-10-25 2009-01-02 Chevron U.S.A. Inc., San Ramon Rostschutzmittel für hochparaffinische Grundschmieröle

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Publication number Priority date Publication date Assignee Title
GB9803367D0 (en) 1998-02-17 1998-04-15 Exxon Research Engineering Co Lubricating grease composition and preparation
US6100226A (en) * 1998-05-20 2000-08-08 The Lubrizol Corporation Simple metal grease compositions
US6063742A (en) * 1999-03-01 2000-05-16 The Lubrizol Corporation Grease compositions
US6482779B2 (en) 2000-03-21 2002-11-19 Nsk Ltd. Lubricating grease composition and rolling apparatus comprising same
JP2001335792A (ja) * 2000-03-21 2001-12-04 Nsk Ltd 潤滑グリース組成物及びそれを用いた転がり軸受、転動装置
DE10254795A1 (de) * 2002-11-22 2004-06-09 Fuchs Europe Schmierstoffe Gmbh Schmierfett enthaltend Polyether-Verbindungen
CN102124089A (zh) * 2008-08-01 2011-07-13 国际壳牌研究有限公司 润滑脂组合物
CN109517644A (zh) * 2018-11-13 2019-03-26 贵州丰达轴承有限公司 一种降噪润滑剂
CN114085694A (zh) * 2021-12-22 2022-02-25 新乡市恒星科技有限责任公司 一种瓦楞辊轴承专用润滑脂及其制备方法

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Publication number Priority date Publication date Assignee Title
DE3379227D1 (en) * 1982-01-21 1989-03-30 Shell Int Research High dropping-point lithium-complex grease having improved anti-noise properties
JPS63309591A (ja) * 1987-06-11 1988-12-16 Nippon Denso Co Ltd グリ−ス組成物
CA2014699A1 (en) * 1989-04-20 1990-10-20 The Lubrizol Corporation Methods for reducing friction between relatively slideable components using metal overbased colloidal disperse systems

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE112006003061T5 (de) 2005-10-25 2009-01-02 Chevron U.S.A. Inc., San Ramon Rostschutzmittel für hochparaffinische Grundschmieröle

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JP3762432B2 (ja) 2006-04-05
JPH10501844A (ja) 1998-02-17
DE69524412D1 (de) 2002-01-17
CA2191481C (en) 2005-06-07
CA2191481A1 (en) 1995-12-28
DE69524412T2 (de) 2002-05-02
EP0765374A1 (de) 1997-04-02
WO1995035355A1 (en) 1995-12-28

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