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EP0668900B1 - Graisses - Google Patents

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Publication number
EP0668900B1
EP0668900B1 EP93924736A EP93924736A EP0668900B1 EP 0668900 B1 EP0668900 B1 EP 0668900B1 EP 93924736 A EP93924736 A EP 93924736A EP 93924736 A EP93924736 A EP 93924736A EP 0668900 B1 EP0668900 B1 EP 0668900B1
Authority
EP
European Patent Office
Prior art keywords
grease
organo
molybdenum
accordance
wear
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
EP93924736A
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German (de)
English (en)
Other versions
EP0668900A1 (fr
EP0668900B2 (fr
Inventor
Gareth Fish
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.)
GKN Technology Ltd
Original Assignee
GKN Technology Ltd
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Application filed by GKN Technology Ltd filed Critical GKN Technology Ltd
Publication of EP0668900A1 publication Critical patent/EP0668900A1/fr
Application granted granted Critical
Publication of EP0668900B1 publication Critical patent/EP0668900B1/fr
Publication of EP0668900B2 publication Critical patent/EP0668900B2/fr
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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
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Definitions

  • This invention relates to greases intended primarily but not exclusively for use in constant velocity joints.
  • Greases consist essentially of a base oil with a thickening agent and other additives may be included to promote specific properties, for example extreme pressure lubricants and anti-oxidants.
  • the thickening agent employed is traditionally a soap, but greases formulated in this way cannot achieve the high performance as required by modern technological demands and more recently greases have been made using organic polymers as a thickening agent, particularly polyureas. However, such greases offer little advantage since whilst achieving lower friction, they promote greater wear than traditional soap greases.
  • US-A-4 536 308 discloses a simple lithium soap grease with an additive composition which consists of 4 to 8 wt % of sulphurised sperm oil substitute, 0.5 to 2.0 wt % of the reaction product of coconut oil and diethanolamine, 2.4 to 5.0 wt % of zinc dialkyldithiophosphate, 0.5 to 2.0 wt % of zinc diamyl-dithiocarbamate and 0.5 to 1.0 wt % of aromatic amine phosphate.
  • WO-A-9 113 955 discloses a complex lithium soap grease containing an organo-metallic compound such as a molybdenum dialkyldithiocarbamate.
  • GB-A-2 255 346 discloses a grease thickened with a diurea and additionally including 0.5 to 3 % by weight of molybdenum sulphide dialkyldithio-carbamate, 0.5 to 3 % by weight of a zinc dithiophosphate extreme pressure additive, 0.5 to 3 % by weight of a sulphur-phosphorus series extreme pressure additive containing no metallic element and having a sulphur content of 10-30 % by weight and a phosphorus content of 0.5-5 % by weight, and 0.5 to 3 % by weight of lead dialkyldithiocarbamate.
  • the object of the invention is to provide an improved grease offering low friction and low wear which is suitable for use in a constant velocity joint, but may also have other applications, and we have discovered that this can be achieved by utilising a lithium-based soap thickener in combination with other specific materials.
  • a grease comprising a base oil and a lithium-based soap thickener in combination with:-
  • greases according to such a formulation may be used as a base grease, together with other conventional additives, such as molybdenum disulphide, in the preparation of a grease composition which in testing and when used in a constant velocity joint provides both low friction and low wear in a manner not achievable by other known grease formulations or other trial formulations differing from the above formulation. It is thought that this combination of properties alises from a synergistic effect obtained by the use of the combination of the organo-sulphur and organo-phosphorus compounds in conjunction with the organo-molybdenum complex and the lithium-based soap.
  • the organo-molybdenum complex may comprise a molybdenum di-thiocarbamate in accordance with the formula or a molybdenum di-thiophosphate according to the formula wherein in both cases
  • the anti-wear/anti-oxidant compound may comprise a zinc dithiophosphate according to the formula
  • the thickener may comprise a simple lithium soap formed from stearic acid or from 12-hydroxystearic acid or from other similar fatty acids, or a lithium complex soap formed from a mixture of such acids. More particularly, the lithium complex soap may comprise a mixture of hydroxy fatty acids and di-acid salts, such as lithium 12-hyroxystearate and lithium azelate.
  • Simple lithium soaps and complex lithium soaps when used in formulations in accordance with the invention appear to behave in substantially the same way, except that where the simple soap is employed the grease will operate only up to temperatures of about 120°C, whereas the complex soaps enable temperatures of up to about 180°C to be sustained.
  • the base oil may comprise a mineral oil or a synthetic oil or a mixture of such oils.
  • the invention also resides in a method of lubricating a constant velocity joint characterised by the use of such a grease, and further in a constant velocity joint packed with such a grease.
  • the base grease comprised a polyalphaolefin containing 10% lithium complex soap thickener consisting of a 60:40 mixture of 12-hydroxystearate and azelate, with the addition of conventional additives such as tackiness agents, corrosion inhibiters and viscosity index improvers.
  • a lithium soap grease in accordance with the invention was made by using the above-mentioned base grease and adding thereto:-
  • a comparative lithium soap grease not in accordance with the invention was made by using the above-mentioned lithium complex base grease and adding thereto:-
  • a further comparison lithium soap grease not in accordance with the invention was made up using the same lithium complex base grease and adding thereto: -
  • Wear in the SRV test was determined by microscopic inspection to obtain a measurement of scar diameter, and a Rank Taylor Hobson Surtronic surface finish measuring machine was employed to determine the depth and cross-section of any scarring. These two measurements were used to calculate wear rate.
  • the term "low wear” as used herein generally indicates that no scar depth was measurable.
  • the grease of Example 3 performed only a little better in terms of co-efficient of friction than prior art grease (A) and not as well as prior art grease (B) and it also did not exhibit the required low wear characteristic.
  • the grease of Example 2 performed somewhat better than prior grease (B) but again did not exhibit the required low wear characteristics.
  • the grease in accordance with Example 1 i.e. in accordance with the invention, not only had an improved co-efficient of friction relative to the other greases tested, but also exhibited low wear characteristics.
  • Figure 2 which shows the surface profile of test samples from the SRV tests using the grease of Examples 1 and 2 at moderate load.
  • the grease of Example 1 in accordance with the invention shows no significant scarring. whereas that of Example 2 shows some scarring.
  • a further lithium soap grease in accordance with the invention was made up using the above-mentioned lithium complex base grease and adding thereto:-
  • a further comparative lithium soap grease not in accordance with the invention was made up as in Example 4 but omitting the tritolylphosphate and substituting half of the stated organo-molybdenum complex by a primary alkyl molybdenum di-thiocarbamate.
  • a further comparative lithium soap grease not in accordance with the invention was made up as in Example 4 but omitting the tritolylphosphate.
  • the greases of Examples 4 and 6 performed significantly better in terms of co-efficient of friction than the grease of Example 5, but only the grease of Example 4 had the required low wear characteristics, as illustrated in Figure 5 which shows the surface profile of test Samples from the SRV tests using greases of Examples 4 and 6 at high load.
  • the grease of Example 6 which is not in accordance with the invention, shows very significant scarring whereas that of Example 4 shows much less scarring.
  • a still further lithium soap grease in accordance with the invention was prepared as in Example 1 but using a sulphurised fatty acid ester instead of the sulphurised synthetic sperm oil.
  • Another blend also substituted trixylenylphosphate for the tritolylphosphate, giving similar results.
  • a still further comparative lithium soap grease not in accordance with the invention was prepared as in Example 2 but replacing half of the stated molybdenum di-thiophosphate by 2-ethylhexyl molybdenum di-thiocarbamate.
  • a still further comparative lithium soap grease not in accordance with the invention was prepared using the above-mentioned lithium complex base grease and adding thereto:-
  • a still further comparative lithium soap grease not in accordance with the invention was prepared using the above-mentioned lithium complex base grease and adding thereto:-
  • Example 8 All performed similarly with regard to co-efficient of friction at only a moderate value. and only that of Example 10 exhibited the required low wear characteristics, but this grease was not considered to provide a sufficiently low co-efficient of friction. However, the grease of Example 7, in accordance with the invention, showed not only a suitably low co-efficient of friction, but also the required low wear characteristic.
  • the base grease comprises a mixture of polybutene and mineral oil containing the lithium-based complex soap thickener, also with the addition of conventional additives as previously mentioned.
  • a grease in accordance with the invention was made using the last-mentioned base grease and adding thereto:
  • a further grease, also in accordance with the invention was made in accordance with Example 11 but with the amounts of the specified additives reduced by 50% whilst retaining the same ratio to one another.
  • results for Example 11 showed slightly higher friction than for Examples 1 and 12 but less than those for Example 2, whereas the results for Example 12 are virtually indistinguishable from those for Examples 1 and 7.

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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)

Abstract

Une graisse essentiellement destinée à être utilisée avec des joints à vitesse constante comprend une huile de base qui peut être une huile minérale, une huile de synthèse ou un mélange de telles huiles, et un épaississant à base de savon de lithium, lequel épaississant peut être un sel de lithium simple ou un sel de lithium complexe, en combinaison avec: (1) un complexe organomolybdique capable de fonctionner comme additif réduisant la friction; (2) un composé antiusure/antioxydant; (3) un additif organosoufré pour améliorer la résistance aux pressions extrêmes; et (4) un additif organophosphoré pour améliorer la résistance aux pressions extrêmes. Il a été trouvé qu'une graisse de cette formule présente une combinaison inattendue de caractéristiques de faible friction et d'usure réduite lorsqu'elle est utilisée dans des joints soumis à une vitesse constante.

Claims (8)

  1. Graisse se composant d'une huile de base et d'un épaississant de savon à base de lithium, combinée :
    (1) à une quantité comprise entre 2 % et 5 % en poids d'un complexe organique avec du molybdène pouvant fonctionner comme un additif réduisant le frottement et sélectionné dans le groupe comprenant les dithiophosphates alkylés de molybdène, les dithiocarbamates alkylés de molybdène et un mélange de ces substances ;
    (2) à une quantité comprise entre 1 % et 2 % en poids d'un composé anti-usure/anti-oxydant comprenant un dithiophosphate de zinc ;
    (3) à une quantité comprise entre 1 % et 2 % en poids d'un additif pour pression extrême à base d'un composé organosulfuré sélectionné dans le groupe comprenant les huiles synthétiques sulfurées de spermaceti, les esters d'acides gras sulfurés, les glycérides d'acides gras sulfurés et un mélange de ces substances ; et
    (4) à une quantité comprise entre 1 % et 2 % en poids d'un additif pour pression extrême à base d'un composé organophosphoré comprenant d'un phosphate de triaryle.
  2. Graisse selon la revendication 1, dont le complexe organique avec du molybdène comprend un dithiocarbamate de molybdène selon la formule :
    Figure 00190001
    où
    X ou Y =
    S ou O
    R =
    un groupe d'alkyle primaire ou secondaire.
  3. Graisse selon la revendication 1, dont le complexe organique avec du molybdène comprend un dithiophosphate de molybdène selon la formule :
    Figure 00200001
    où
    X ou Y =
    S ou O
    R =
    un groupe d'alkyle primaire ou secondaire.
  4. Graisse selon la revendication 1, dont le composé anti-usure/anti-oxydant comprend un dithiophosphate de zinc selon la formule :
    Figure 00200002
    où
    R =
    un alkyle secondaire.
  5. Graisse selon la revendication 1, dont l'épaississant est sélectionné dans le groupe comprenant les savons simples et complexes à base de lithium.
  6. Graisse selon la revendication 1, dont l'huile de base est sélectionnée dans le groupe comprend les huiles minérales, les huiles synthétiques et un mélange de ces huiles.
  7. Procédé de lubrification d'un joint à vitesse constante, caractérisé par l'utilisation d'une graisse selon l'une quelconque des revendications précédentes.
  8. Joint à vitesse constante utilisé avec une graisse selon l'une quelconque des revendications 1 à 6.
EP93924736A 1992-11-14 1993-11-10 Graisses Expired - Lifetime EP0668900B2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB9223945 1992-11-14
GB929223945A GB9223945D0 (en) 1992-11-14 1992-11-14 Greases
PCT/GB1993/002313 WO1994011470A1 (fr) 1992-11-14 1993-11-10 Graisses

Publications (3)

Publication Number Publication Date
EP0668900A1 EP0668900A1 (fr) 1995-08-30
EP0668900B1 true EP0668900B1 (fr) 1998-10-07
EP0668900B2 EP0668900B2 (fr) 2002-05-29

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EP93924736A Expired - Lifetime EP0668900B2 (fr) 1992-11-14 1993-11-10 Graisses

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EP (1) EP0668900B2 (fr)
DE (1) DE69321481T3 (fr)
GB (2) GB9223945D0 (fr)
WO (1) WO1994011470A1 (fr)

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Also Published As

Publication number Publication date
DE69321481D1 (de) 1998-11-12
GB9223945D0 (en) 1993-01-06
DE69321481T2 (de) 1999-05-27
DE69321481T3 (de) 2002-09-05
GB2287715A (en) 1995-09-27
EP0668900A1 (fr) 1995-08-30
EP0668900B2 (fr) 2002-05-29
GB2287715B (en) 1996-08-21
WO1994011470A1 (fr) 1994-05-26
GB9508436D0 (en) 1995-06-14

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