EP0117454B1 - Composition de graisse lubrifiante, sa préparation et son application - Google Patents

Composition de graisse lubrifiante, sa préparation et son application Download PDF

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Publication number
EP0117454B1
EP0117454B1 EP84101018A EP84101018A EP0117454B1 EP 0117454 B1 EP0117454 B1 EP 0117454B1 EP 84101018 A EP84101018 A EP 84101018A EP 84101018 A EP84101018 A EP 84101018A EP 0117454 B1 EP0117454 B1 EP 0117454B1
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EP
European Patent Office
Prior art keywords
grease composition
composition according
lubricating grease
oil
polyurea
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
Application number
EP84101018A
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German (de)
English (en)
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EP0117454A1 (fr
Inventor
Hans Schreiber
Norbert Matzat
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.)
Optimol-Olwerke GmbH
Original Assignee
Optimol-Olwerke GmbH
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
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Application filed by Optimol-Olwerke GmbH filed Critical Optimol-Olwerke GmbH
Publication of EP0117454A1 publication Critical patent/EP0117454A1/fr
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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
    • C10M169/04—Mixtures of base-materials 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
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • 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
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/042—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds between the nitrogen-containing monomer and an aldehyde or ketone
    • 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
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/043—Mannich bases

Definitions

  • the invention relates to a grease composition based on a larger proportion of mineral or synthetic oil as the base oil and a smaller proportion of polyurea as a thickener.
  • the invention has for its object to reduce or eliminate these disadvantages of the previously known oil-based greases with polyureas as thickeners.
  • a grease composition based on a larger proportion of mineral or synthetic oil as base oil and a smaller proportion of a polyurea compound as a thickener and conventional additives, which is characterized in that, as polyurea, it is the reaction product of an isocyanate with at least 3 isocyanate groups in the Contains molecule with a long-chain, straight-chain or branched aliphatic monoamine.
  • the polyureas used according to the invention are crosslinked high-molecular products which have been mechanically comminuted.
  • the amine component preferably consists predominantly of the monoamines with 16 to 24 carbon atoms, but smaller portions of monoamines with shorter chains down to 10 carbon atoms may also be present, but an amount of 10% of the total amine should not be exceeded . Small amounts of diamines can also be added, an amount of about 5% should not be exceeded.
  • long-chain aliphatic monoamine means compounds with more than 14 carbon atoms, preferably those with 16 to 24 carbon atoms, and mixtures thereof. Longer-chain monoamines are also technically useful for the invention, but are currently difficult to obtain economically.
  • the monoamine can be a saturated fatty amine or contain one or more olefinic double bonds.
  • Straight-chain or branched, aliphatic amines can be used.
  • Particularly preferred for monounsaturated fatty amines are those with 16 to 20 C atoms, more preferably an alkenylamine with 18 C atoms (oleylamine), on the one hand, and for saturated aliphatic alkylamines those with 18 to 24 C atoms, more preferably with 20 up to 22 carbon atoms, on the other hand.
  • Each of these preferred embodiments of the polyurea has special properties with regard to compatibility with additives.
  • Both aliphatic polyisocyanates, such as Desmodur N, which contain tri-, tetra- and higher polyisocyanates, and aromatic polyisocyanates, such as Desmodur R, can be used.
  • the latter which is chemically p, p ', p "-triphenylmethane triisocyanate in the form of a 20% solution in methylene chloride, has been found to be particularly suitable within the scope of the invention.
  • the suitability of a special polyisocyanate within the scope of the invention can be found in the rest can easily be determined by simple preliminary tests.
  • the grease composition according to the invention contains the polyurea in an amount sufficient to achieve the desired thickening effect. Good results are generally obtained with additions of between 3 and 45% by weight of polyurea, based on the base oil. The best results are generally obtained at levels between 8 and 15%.
  • mineral oil and synthetic oil come into consideration as base oil.
  • Naphthenic base oils are preferred.
  • Paraffin-based base oils can also be used.
  • polyureas are preferably used as thickeners, in which the monoamine component is as long-chain as possible within the scope taught by the invention.
  • the lubricating grease compositions according to the invention can contain both oil-soluble and non-oil-soluble additives in order, for example, to improve the high-pressure properties, the wear behavior and the oxidation resistance.
  • These lubricant additives are known to the person skilled in the art and do not require any further explanation here unless special considerations in connection with the various possible modification forms of the polyurea used according to the invention need to be taken into account.
  • Solid additives with high-pressure and / or anti-wear-improving properties are primarily graphite and the lubricating metal sulfides, either alone or in combination with activity enhancers.
  • graphite and molybdenum disulfide and their mixtures are preferred in the context of the invention.
  • Suitable effect amplifiers are e.g. Metal oxides, hydroxides, phosphates or fluorides.
  • These non-oil-soluble additives are particularly suitable in combination with polyureas, the monoamine component of which is in the longer-chain range, that is to say between about 18 to 24 carbon atoms, preferably 20 to 22 carbon atoms. However, they can be used in all polyureas to be used in the context of the invention.
  • the amount of these non-oil-soluble additives is generally between 0.5 and 10% by weight, based on the total fat composition, an addition of 2 to 6% is particularly preferred. If the specified quantities are exceeded, there is no improvement in the properties which would be adequate for the increased costs; if the limit values are undershot, the desired properties are no longer obtained. From the point of view of the best possible fatigue strength, friction properties and an acceptable price, particularly satisfactory results are obtained with a 2 to 4% addition of non-oil-soluble additive and usually oil-soluble antioxidant.
  • a particular advantage of the grease composition according to the invention is the excellent compatibility with oil-soluble additives, in particular also oil-soluble high-pressure and anti-wear additives.
  • oil-soluble additives in particular also oil-soluble high-pressure and anti-wear additives.
  • the highly effective oil-soluble high-pressure and anti-wear additives proved to be unsuitable, since they led to rapid degradation of the polyureas which were prepared with diisocyanates.
  • safe oil-soluble additives only gave unsatisfactory properties of the grease composition.
  • the particularly effective oil-soluble additives can also be used without having negative effects on the polyurea component in continuous operation.
  • those embodiments of the grease composition according to the invention in which the amine component of the polyurea is unsaturated and in the lower range of the chain length in question have proven to be particularly suitable.
  • the oil-soluble additives are generally used in amounts between 3 and 20% by weight, based on the total grease composition. An addition of between about 5 and 12% by weight is preferred.
  • Another object of the invention is the method for producing the grease composition described in more detail above. This process is characterized in that a long-chain aliphatic monoamine or a mixture of such amines is dissolved in the base oil, polyisocyanate is added, the mixture is heated to a temperature of at least 160 ° C. until gelation occurs, the gelled product is mechanically minced and the additives and add further base oil if necessary.
  • the method is based on the mineral or synthetic oil or a mixture of such oils which is to be used as the base oil for the grease composition. If it is a mixture of oils, the process can also be carried out with only one oil component and the further oil component can be added later. It is also possible to use a smaller proportion of base oil in the process than is required for the desired composition with regard to the amount of polyurea. The amount of oil only has to be sufficient to completely dissolve the amine.
  • the aliphatic monoamine or mixture thereof is expediently introduced into the base oil in the molten state in order to facilitate the dissolution, the dissolution being able to be facilitated by stirring and heating.
  • a suitable amount of the selected triisocyanate is added thereafter or simultaneously. Quantities in which 1/2 to 4 isocyanate groups are available per amine group are generally suitable. In special cases, these conditions can also be exceeded or fallen short of.
  • the mixture obtained is heated until several recognizable reaction stages are run through and finally gelation occurs.
  • the temperature required depends on the reaction components used and any additives present and is generally above 160 ° C., preferably above 200 ° C. Heating above 240 ° C is generally not required, but can be used.
  • the gelled mass is then mechanically comminuted, it being possible to use the known comminution methods and devices.
  • the gel is expediently ground in a colloid mill.
  • the additives are then added, and, if appropriate, the remaining amount of base oil.
  • Preferred amine for the process is oleylamine or a saturated alkylamine or alkylamine mixture having 20 to 22 carbon atoms.
  • the statements made above apply with regard to the preferred polyisocyanate.
  • the grease composition according to the invention is characterized by improved mechanical stability, in particular in combination with oil-soluble additives, i.e. oil-soluble high-pressure and anti-wear additives. So far, however, it has only been possible to obtain satisfactory lubricating greases based on lubricating oil with polyurea as a thickener with good high-pressure properties when using non-oil-soluble high-pressure additives.
  • oil-soluble additives i.e. oil-soluble high-pressure and anti-wear additives.
  • the lubricating grease composition according to the invention is even superior to the best known lithium greases in terms of the achievable high-pressure properties and wear resistance, and at the same time allows the permanent operating temperature, which is in the range from 80 to 110 ° C. and briefly up to 135 ° C. for lithium greases, to be increased to a continuous operating temperature of 150 to 160 ° C, for a short time beyond that too. This corresponds to a very significant improvement in service life and temperature resistance.
  • the lubricating grease composition according to the invention is not inferior to the best commercially available lubricating greases even in the low temperature range down to well below minus 30 ° C. It thus has a combination of properties that have not previously been known for commercially available products.
  • the best known lithium greases can be used to achieve 20 to 25 million rollovers at 50 ° C in particularly difficult conditions, such as those found in homokinetic joints and simulated in cardan shaft test benches.
  • the lubricating grease compositions according to the invention at least 30 million rollovers can still be achieved on such cardan shaft test benches at temperatures of 150 to 160 ° C.
  • FIG. 1 of the attached drawing The improved properties achieved according to the invention can be illustrated by FIG. 1 of the attached drawing.
  • Example 1 shows a test sheet which was obtained with the grease composition according to the invention from Example 1 on the commercially available lubricant tester SRV, which is sold by the applicant and which is described in ant «drive technology 19 (1980) No. 1-2.
  • the lubricant composition was subjected to a load increasing from 50 to 1000 Newtons under the specified operating conditions, without the lubricating effectiveness collapsing. This means that the flow limit of the metal is reached in the surface roughness without the lubricating effect of the grease composition according to the invention being lost.
  • 4000 g naphthenic base oil of 100 centistokes (10- 4 m 2 / sec) at 40 ° C, viscosity index approx. 45 are mixed with 400 g saturated monofatty amine with 20 to 22 C atoms in the molten state and with 1200 g a 20% solution of p, p ', p "-triphenvimethane triisocyanate in methylene chloride, heated with stirring until the methylene chloride has evaporated and then further heated until reached 240 ° C. As soon as the mixture has gelled, it is cooled, comminuted and in Finely ground in a colloid mill, this gives a base fat which is classified as penetration class 3 according to DIN 51818.
  • an oil-soluble additive according to DE-AS 1 954 452 was added, which contained Pb and Mo dialkyldithiophosphate, a metal-free sulfur-phosphorus compound and an epoxide of an ester of an unsaturated fatty acid with an alkanol.
  • Example 2 The procedure of Example 2 is repeated, but instead of the oil-soluble additives, the additives of Example 1 are added in the amount specified there. 5 of the drawing in the form of test sheet 8254 shows the results of the test on the SRV device.
  • the minimum coefficient of friction is 0.085 ⁇
  • the diameter of the wear ball is 0.50 mm at 300 Newton load.
  • Example 2 As described in Example 1, a grease was produced, but 800 g was used instead of 1200 g of isocyanate solution and 3% was used instead of 0.5% antioxidant.
  • the grease obtained in this way was examined on a cardan shaft test bench.
  • the joint was heated to an ambient temperature of 75 ° C and then loaded at 1200 revolutions, 8 ° bending angle and 320 Nm.
  • a rating scale from 1 to 6, in which 1 represents the best and 6 the worst value, the best serial grease based on lithium soap available on the market gave a rating of 4.3 ⁇ 1 and an outside temperature of 103 ⁇ 0 ° C, which corresponds to an internal joint temperature of 15 to 130 ° C.

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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 (16)

1. Composition de graisse lubrifiante à base d'une proportion relativement grande d'une huile minérale ou de synthèse en tant qu'huile de base et d'une proportion relativement plus petite d'un composé polycarbamide en tant qu'épaississant ainsi que des additifs usuels, caractérisée en ce qu'elle contient en tant que polycarbamide le produit réactionnel d'un isocyanate ayant au minimum trois groupes isocyanates dans la molécule avec une monoamine ramifiée ou linéaire à chaîne longue aliphatique.
2. Composition de graisse lubrifiante selon la revendication 1, caractérisée en ce qu'elle contient 3 à 45% en poids de polycarbamide, rapportés à l'huile de base.
3. Composition de graisse lubrifiante selon la revendication 1 ou 2, caractérisée en ce que le polycarbamide est à base de triisocyanate de triphenyl- méthane.
4. Composition de graisse lubrifiante selon l'une des revendications précédentes, caractérisée en ce qu'elle contient un polycarbamide comportant une alcoylène-amine ayant 18 atomes de C en tant que composant amine.
5. Composition de graisse lubrifiante selon l'une des revendications 1 à 3, caractérisée en ce qu'elle contient un polycarbamide ayant une alcoyle-amine saturée en C20 à C22 en tant que composant amine.
6. Composition de graisse lubrifiante selon la revendication 4 ou 5, caractérisée en ce qu'elle contient des additifs haute pression ou/et anti-usure solubles dans l'huile.
7. Composition de graisse lubrifiante selon la revendication 6, caractérisée en ce qu'elle contient 3 à 20% en poids d'additifs.
8. Composition de graisse lubrifiante selon la revendication 4 ou 5, caractérisée en ce qu'elle contient des additifs à haute pression ou anti-usure non solubles dans l'huile.
9. Composition de graisse lubrifiante selon la revendication 8, caractérisée en ce qu'elle contient du graphite ou/et un sulphure de métal à pouvoir lubrifiant en tant qu'additif haute pression ou anti-usure.
10. Composition de graisse lubrifiante selon la revendication 8 ou 9, caractérisée en ce qu'elle contient 0,5 à 10% en poids d'additifs.
11. Composition de graisse lubrifiante selon l'une des revendications précédentes, caractérisée en ce qu'elle contient 2 à 6% en poids d'additifs non solubles dans l'huile ou 3 à 12% en poids d'additifs solubles dans l'huile.
12. Procédé pour la préparation d'une composition de graisse lubrifiante selon l'une des revendications 1 à 11, caractérisé en ce que l'on dissout dans l'huile de base une amine à chaîne longue aliphatique ou un mélange de telles amines, que l'on ajoute de l'isocyanate comportant au minimum 3 groupes isocyanates dans la molécule, que l'on chauffe le mélange à une température d'au minimum 160°C, qu'une gélification se produit, que l'on divise finement le produit gélifié par un moyen mécanique et que l'on ajoute les additifs et éventuellement de l'huile de base supplémentaire.
13. Procédé selon la revendication 12, caractérisé en ce que l'on ajoute 1/2 à 4 équivalents de groupes isocyanates par groupe amine.
14. Procédé selon le revendication 12 ou 13, caractérisé en ce qu'en tant qu'amine on utilise une oléylamine ou une alcoyle-amine saturée ou un mélange d'alcoyle-amine ayant 20 à 22 atomes de C.
15. Procédé selon l'une des revendications 12 à 14, caractérisé en ce qu'en tant que triisocyanate on utilise du triisocyanate de triphénylméthane.
16. Utilisation d'une composition de graisse lubrifiante selon les revendications 1 à 11, dans des articulations homocinétiques.
EP84101018A 1983-02-02 1984-02-01 Composition de graisse lubrifiante, sa préparation et son application Expired EP0117454B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19833303442 DE3303442A1 (de) 1983-02-02 1983-02-02 Schmierfettzusammensetzung, ihre herstellung und verwendung
DE3303442 1983-02-02

Publications (2)

Publication Number Publication Date
EP0117454A1 EP0117454A1 (fr) 1984-09-05
EP0117454B1 true EP0117454B1 (fr) 1986-08-06

Family

ID=6189815

Family Applications (2)

Application Number Title Priority Date Filing Date
EP84900713A Pending EP0134234A1 (fr) 1983-02-02 1984-02-01 Composition de graisses, sa fabrication et son utilisation
EP84101018A Expired EP0117454B1 (fr) 1983-02-02 1984-02-01 Composition de graisse lubrifiante, sa préparation et son application

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP84900713A Pending EP0134234A1 (fr) 1983-02-02 1984-02-01 Composition de graisses, sa fabrication et son utilisation

Country Status (6)

Country Link
US (1) US4692255A (fr)
EP (2) EP0134234A1 (fr)
CA (1) CA1229332A (fr)
DE (2) DE3303442A1 (fr)
ES (1) ES8503368A1 (fr)
WO (1) WO1984003100A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6346299A (ja) * 1986-01-16 1988-02-27 Ntn Toyo Bearing Co Ltd プランジング型等速ジョイント用グリース
DE3918107A1 (de) * 1989-06-02 1990-12-06 Klueber Lubrication Schmierfettzusammensetzung
CA2093029C (fr) * 1992-04-14 2003-07-29 Jon C. Root Lubrifiants, notamment compositions pour graisse lubrifiante, pour joints universels a vitesse constante
JP4427195B2 (ja) * 2001-01-26 2010-03-03 Ｎｔｎ株式会社 自動車用グリース封入軸受
JP2009529597A (ja) * 2006-03-14 2009-08-20 ハンツマン・インターナショナル・エルエルシー ジイソシアネートとモノアミンから製造される組成物およびその製造方法
US9012384B2 (en) 2010-07-30 2015-04-21 Chevron U.S.A. Inc. Method of preparing greases
US8889604B2 (en) 2010-07-30 2014-11-18 Chevron U.S.A. Inc. Method of preparing greases

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2832739A (en) * 1955-06-13 1958-04-29 Standard Oil Co Ureido thickened greases
US2925387A (en) * 1958-07-21 1960-02-16 Standard Oil Co Method of preparing ureido grease-thickener concentrate and lubricating greases containing same
US3243372A (en) * 1961-01-24 1966-03-29 Chevron Res Greases thickened with polyurea
US3242210A (en) * 1965-03-16 1966-03-22 Chevron Res Polyureas
US3401027A (en) * 1967-04-10 1968-09-10 Chevron Res Light hydrocarbon liquids containing a jellifying agent comprising polyureas
US3879305A (en) * 1973-03-26 1975-04-22 Mobil Oil Corp Grease thickened with oxygen-linked or sulfur-linked polyureas

Also Published As

Publication number Publication date
CA1229332A (fr) 1987-11-17
WO1984003100A1 (fr) 1984-08-16
US4692255A (en) 1987-09-08
ES529387A0 (es) 1985-02-16
ES8503368A1 (es) 1985-02-16
DE3303442A1 (de) 1984-08-16
DE3460405D1 (en) 1986-09-11
EP0117454A1 (fr) 1984-09-05
EP0134234A1 (fr) 1985-03-20

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