EP0433405A1 - Lubricating grease composition. - Google Patents

Lubricating grease composition.

Info

Publication number
EP0433405A1
EP0433405A1 EP90908203A EP90908203A EP0433405A1 EP 0433405 A1 EP0433405 A1 EP 0433405A1 EP 90908203 A EP90908203 A EP 90908203A EP 90908203 A EP90908203 A EP 90908203A EP 0433405 A1 EP0433405 A1 EP 0433405A1
Authority
EP
European Patent Office
Prior art keywords
base oil
thickener
grease composition
lubricating grease
ester
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
EP90908203A
Other languages
German (de)
French (fr)
Other versions
EP0433405B1 (en
Inventor
Edwin Seubert
Dieter Sohn
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.)
Klueber Lubrication Muenchen GmbH and Co KG
Original Assignee
Klueber Lubrication Muenchen GmbH and Co KG
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Filing date
Publication date
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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
    • C10M169/02—Mixtures of base-materials and thickeners
    • 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
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/32—Esters
    • C10M105/36—Esters of polycarboxylic acids
    • 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
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/24—Lubricating compositions characterised by the thickener being a macromolecular compound 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
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
    • C10M2207/2825—Esters of (cyclo)aliphatic oolycarboxylic acids used as base 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/284—Esters of aromatic monocarboxylic acids
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/285—Esters of aromatic polycarboxylic acids
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/285—Esters of aromatic polycarboxylic acids
    • C10M2207/2855—Esters of aromatic polycarboxylic acids used as base 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/34—Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
    • 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 composed of a base oil and a smaller proportion of a thickener based on a polyurea compound, and also conventional additives.
  • Such lubricants are e.g. known from DE-OS 33 03 442, wherein the base oil is a mineral or synthetic oil, such as a naphthenic or paraffin-based base oil and the thickener is the reaction product of an isocyanate with at least 3 isocyanate groups in the molecule with a long-chain aliphatic monoamine, preferably with 16 to 24 carbon atoms.
  • the base oil is a mineral or synthetic oil, such as a naphthenic or paraffin-based base oil
  • the thickener is the reaction product of an isocyanate with at least 3 isocyanate groups in the molecule with a long-chain aliphatic monoamine, preferably with 16 to 24 carbon atoms.
  • Such grease compositions can be used for long-term use temperatures of 150-160 ° C.
  • compositions which each contain an ester as the base oil and have a consistency with a penetration of 220 to 385 at 0.1 mm and where the thickener consists of an aromatic mono- or diisocyanate and an alkyl, alkenyl radical with 8 to 22 C- Atoms or aryl radicals composed of 6 to 10 carbon atoms have been found to be particularly silencing, the property being particularly important in the case of mechanically moving parts in electronic apparatus, such as turntables, tapes and video equipment, etc.
  • Lubricating grease preparations of this type are suitable for roller bearings which have to withstand temperatures of up to 180 ° C.
  • the lubricating grease composition according to the invention consisting of a base oil and a smaller proportion of a thickening agent based on a polyurea compound and conventional additives is characterized in that the base oil is an ester of an aromatic di-, tri- or tetracarboxylic acid with one or more C ..- C, Q -alkanols and the thickener is the reaction product of a compound of the general formula
  • the mixture of base oil and thickener has a consistency with a penetration of 220-385, 0.1 mm.
  • Such greases correspond to NLGI class 3 to 0 according to DIN ISO 2137.
  • the preferred base oils have a viscosity of 18 to 400 mm 2 / s at 40 ° C.
  • Lubricants are preferably used in which the base oil is a C 1 -C 4 -alcohol ester of phthalic acid, trimellitic acid or pyromellitic acid and the thickener is the reaction product of a methylene-bis-phenyl isocyanate or tolylene diisocyanate such as a mixture of 2. 4- and 2,6-tolylene diisocyanate, with a C to C __ alkylamine or A inen or naphthylamine.
  • the additives used against corrosion, oxidation and for protection against metal influences which act as chelate compounds, radical scavengers, UV converters and the like, are known per se and are customary in the trade.
  • the noise test is carried out by means of a test arrangement which is particularly suitable for this purpose, a suitable roller bearing having a rotational speed of 1800 min " being run.
  • the noise is measured directly on the outer ring of the rolling bearing by means of an accelerometer.
  • the vibrations recorded by the device are divided into three frequency ranges (low 50 - 300 Hz, medium 300 - 1800 Hz, high 1800 - 10000 Hz). In addition, maximum peaks are also registered.
  • the measured values are evaluated by a computer and referenced to the values which were measured with a reference lubricant. Relative values are obtained in this way compared to the reference value, which is fixed at 100%.
  • the lubricant preparation according to the invention shows values in all areas of around 100% compared to a lubricant made from mineral oil and polyurea, which shows peak values of up to 368%.
  • the fat is homogenized by repeated rolling on a three-roll mill. This homogenization process is of particular importance for the noise behavior. In this way, a grease of NLGI class 0 according to DIN ISO 2137 is obtained. This fat obtained in this way is tested on a noise test bench, which differentiates according to three frequency bands and maximum peaks.
  • Example 2 In 839.5 g of an ester oil consisting of an ester the pyro ellitic acid and an isomeric C-8 alcohol, diisocyanate and amine are reacted as in Example 2. Implementation, additives and homogenization take place in the same way as in Example 1.
  • Noise behavior of the lubricants of Examples 1 to 3 in 3 frequency ranges (1) with maximum peak values (2) or (3).
  • Fig. 2 - the graphical representation of the noise behavior of a comparative lubricant according to the prior art in three frequency ranges (1), (2) and with the maximum peak value (4).
  • Table 1 the numerical statistical evaluation of the lubricant noise test according to FIG. 1 for examples 1 to 3 and
  • Table 2 the same evaluation for the comparison fat according to FIG. 2.

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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)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Lubricants (AREA)
  • Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Steroid Compounds (AREA)
  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Cette graisse lubrifiante contient une huile de base et une proportion moins importante d'un épaississant à base d'un composé polycarbamide, ainsi que les additifs habituels. L'huile de base est l'ester d'un acide dicarboxylique, tricarboxylique ou tétracarboxylique aromatique avec un ou plusieurs alcanols C7-C18. L'épaississant est un produit de la réaction entre un composé correspondant à la formule A(B)n (I) et une amine correspondant à la formule H2N-R (II), où A = CH4-n, B = résidu mono-isocyanate ou di-isocyanate, n = 1 à 3, R = résidu alkyle ou alcényle avec 8 à 22 atomes de C ou résidu aryle avec 6 à 10 atomes de C. Le mélange d'huile de base et d'épaississant a une consistance dont la pénétration est de 220 à 385, 0,1 mm.This lubricating grease contains a base oil and a lower proportion of a thickener based on a polycarbamide compound, as well as the usual additives. The base oil is the ester of an aromatic dicarboxylic, tricarboxylic or tetracarboxylic acid with one or more C7-C18 alkanols. The thickener is a product of the reaction between a compound corresponding to the formula A (B) n (I) and an amine corresponding to the formula H2N-R (II), where A = CH4-n, B = mono- residue isocyanate or di-isocyanate, n = 1 to 3, R = alkyl or alkenyl residue with 8 to 22 C atoms or aryl residue with 6 to 10 C atoms. The mixture of base oil and thickener has a consistency whose penetration is from 220 to 385, 0.1 mm.

Description

Schmierfet ZusammensetzungGrease composition
Beschreibungdescription
Die Erfindung betrifft eine Schmierfettzusammeπset- zung aus einem Grundöl und einem kleineren Anteil eines Verdickungsmittels auf Basis einer Polyharn- stoffVerbindung, sowie üblichen Additiven.The invention relates to a grease composition composed of a base oil and a smaller proportion of a thickener based on a polyurea compound, and also conventional additives.
Derartige Schmiermittel sind z.B. aus der DE-OS 33 03 442 bekannt, wobei das Grundöl ein Mineral¬ oder Syntheseöl, wie ein naphthenbasisches oder pa¬ raffinbasisches Grundöl und das Verdickungsmittel das Reaktionsprodukt eines Isocyanats mit mindestens 3 Isocyanatgrupper im Molekül mit einem langketti- gen aliphatischen Monoamin, vorzugsweise mit 16 bis 24 C-Atomen ist.Such lubricants are e.g. known from DE-OS 33 03 442, wherein the base oil is a mineral or synthetic oil, such as a naphthenic or paraffin-based base oil and the thickener is the reaction product of an isocyanate with at least 3 isocyanate groups in the molecule with a long-chain aliphatic monoamine, preferably with 16 to 24 carbon atoms.
Solche Schmierfettzusammensetzungen sind für Dauer¬ einsatztemperaturen von 150 - 160 °C brauchbar.Such grease compositions can be used for long-term use temperatures of 150-160 ° C.
Ähnliche Zusammensetzungen, die jedpch einen Ester als Grundöl enthalten und eine Konsistenz mit einer Penetration von 220 bis 385 bei 0,1mm aufweisen und wobei das Verdickungsmittel aus einem aromatischen Mono- oder Diisocyanat und einem A_kyl-, Alkenyl- rest mit 8 bis 22 C-Atomen oder Arylrest mit 6 bis 10 C-Atomen zusammengesetzt ist, wurde als besonders ge: äuschdämpfend aufgefunden, wobei die Eigenschaft insbesondere bei mechanisch bewegten Teilen in elek¬ tronischen Apparaten, wie Plattenspielern, Tonband- und Videogeräten usw. von Bedeutung ist. Insbesondere sind derartige Schmierfettzubereitungen bei Wälz¬ lagern geeignet, die Temperaturen bis 180 °C auszu¬ halten haben.Similar compositions which each contain an ester as the base oil and have a consistency with a penetration of 220 to 385 at 0.1 mm and where the thickener consists of an aromatic mono- or diisocyanate and an alkyl, alkenyl radical with 8 to 22 C- Atoms or aryl radicals composed of 6 to 10 carbon atoms have been found to be particularly silencing, the property being particularly important in the case of mechanically moving parts in electronic apparatus, such as turntables, tapes and video equipment, etc. In particular Lubricating grease preparations of this type are suitable for roller bearings which have to withstand temperatures of up to 180 ° C.
Die erfindungsgemäße Schmierfettzusammensetzung aus einem Grundöl und einem kleineren Anteil eines Ver- dicküngsmittels auf Basis einer Polyharnstoffver- bindung sowie üblichen Additiven, ist dadurch gekenn¬ zeichnet, daß das Grundöl ein Ester einer aromati¬ schen Di-, Tri- oder Tetracarbonsäure mit einem oder mehreren C..-C, Q-Alkanolen und das Verdickungsmittel das Reaktionsprodukt einer Verbindung der allgemeinen FormelThe lubricating grease composition according to the invention consisting of a base oil and a smaller proportion of a thickening agent based on a polyurea compound and conventional additives is characterized in that the base oil is an ester of an aromatic di-, tri- or tetracarboxylic acid with one or more C ..- C, Q -alkanols and the thickener is the reaction product of a compound of the general formula
A(B)nA (B) n
und einem A in der allgemeinen Formel H„N-R ist, wobei in den Formelnand an A in the general formula H "N-R, wherein in the formulas
b aromatischer Mono- oder Diisocyanatrest n 1 - 3 R Alkyl- oder Alkenylrest mit 8 bis 22-C-Atomen oder Arylrest mit 6 bis 10-C-Atomen b aromatic mono- or diisocyanate residue n 1 - 3 R alkyl or alkenyl residue with 8 to 22 C atoms or aryl residue with 6 to 10 C atoms
ist, und wobei das Gemisch aus Grundöl und Verdik- kungsmittel eine Konsistenz mit einer Penetration von 220 - 385, 0,1mm aufweist.and the mixture of base oil and thickener has a consistency with a penetration of 220-385, 0.1 mm.
Solche Schmierfette entsprechen der NLGI-Klasse 3 bis 0 nach DIN ISO 2137. Die bevorzugten Grundöle haben eine Viskosität von 18 bis 400 mm2/s bei 40 °C. Bevorzugt werden Schmierstoffe eingesetzt, bei denen das Grundöl ein C„ bis C, ,-Alkoholester der Phthal- säure, Trimellithsäure oder Pyromellithsäure ist und das Verdickungsmittel das Umsetzungsprodukt ei¬ nes Methylen-bis-phenylisocyanats oder Toluylendi- isocyanats wie einem Gemisch von 2,4- und 2,6-To- luylendiisocyanat, mit einem C, bis C__-Alkylamin oder A inen bzw. Naphtylamin darstellt.Such greases correspond to NLGI class 3 to 0 according to DIN ISO 2137. The preferred base oils have a viscosity of 18 to 400 mm 2 / s at 40 ° C. Lubricants are preferably used in which the base oil is a C 1 -C 4 -alcohol ester of phthalic acid, trimellitic acid or pyromellitic acid and the thickener is the reaction product of a methylene-bis-phenyl isocyanate or tolylene diisocyanate such as a mixture of 2. 4- and 2,6-tolylene diisocyanate, with a C to C __ alkylamine or A inen or naphthylamine.
Die verwendeten Additive gegen Korrosion, Oxydation und zum Schutz gegen Metalleinflüsse, die als Che- latverbindungen, Radikalfänger, UV-Umwandler und dergleichen wirken, sind an sich bekannt und han¬ delsüblich.The additives used against corrosion, oxidation and for protection against metal influences, which act as chelate compounds, radical scavengers, UV converters and the like, are known per se and are customary in the trade.
Die Geräuschprüfung wird mittels einer besonders hierfür geeigneten Versuchsanordnung durchgeführt, wobei ein geeignetes Wälzlager mit Umdrehungszahlen von 1800 min" laufen gelassen wird.The noise test is carried out by means of a test arrangement which is particularly suitable for this purpose, a suitable roller bearing having a rotational speed of 1800 min " being run.
Das Geräusch wird mittels eines Beschleunigungsauf¬ nehmers direkt am Außenring des Wälzlagers gemessen. Die vom Gerät aufgezeichneten Schwingungen werden in drei Frequenzbereiche (low 50 - 300 Hz, medium 300 - 1800 Hz, high 1800 - 10000 Hz) aufgeteilt. Zusätzlich werden auch maximale Spitzenwerte (peaks) registriert .The noise is measured directly on the outer ring of the rolling bearing by means of an accelerometer. The vibrations recorded by the device are divided into three frequency ranges (low 50 - 300 Hz, medium 300 - 1800 Hz, high 1800 - 10000 Hz). In addition, maximum peaks are also registered.
Die gemessenen Werte werden von einem Rechner aus¬ gewertet und auf die Werte, welche mit einem Refe¬ renz-Schmiermittel gemessen wurden, bezogen. Man erhält so Relativwerte, im Vergleich zum Refe¬ renzwert, welcher gleich 100 % festgelegt ist. Die erfindungsgemäße Schmiermittelzubereitung zeigt hier in allen Bereichen Werte um 100 % gegenüber einem Schmiermittel aus Mineralöl und Polyharnstoff, wel¬ ches Spitzenwerte bis 368 % zeigt.The measured values are evaluated by a computer and referenced to the values which were measured with a reference lubricant. Relative values are obtained in this way compared to the reference value, which is fixed at 100%. The lubricant preparation according to the invention shows values in all areas of around 100% compared to a lubricant made from mineral oil and polyurea, which shows peak values of up to 368%.
Die Erfindung wird durch die folgenden Beispiele erläutert:The invention is illustrated by the following examples:
Beispiel 1:Example 1:
In 789,5 g eines Esteröles, bestehend aus einem Ester der Phthalsäure und einem isomeren C. ,-Alkohol, wer¬ den 97 g eines Gemisches aus 2,4- und 2,6-Toluylen- diisocyanatIn 789.5 g of an ester oil consisting of an ester of phthalic acid and an isomeric C.I. alcohol, 97 g of a mixture of 2,4- and 2,6-tolylene diisocyanate are added
(A = CH,, π = 1, B = aromatisches Diisocyanat)(A = CH ,, π = 1, B = aromatic diisocyanate)
mit 103 g Anilin (R = Arylrest mit 6-C-Atomen) um¬ gesetzt. Nachdem die exotherme Reaktion abgeschlos¬ sen ist, wird der Sud auf 160 °C aufgeheizt. Wäh¬ rend des Abkuhlens werden 5 g eines handelsüblichen Antioxidants, 5 g eines handelsüblichen Korrosions¬ schutzmittels und 0,5 g eines handelsüblichen Me- talldesaktivators zugesetzt.with 103 g of aniline (R = aryl radical with 6 carbon atoms). After the exothermic reaction is complete, the brew is heated to 160 ° C. 5 g of a commercially available antioxidant, 5 g of a commercially available corrosion protection agent and 0.5 g of a commercially available metal deactivator are added during the cooling.
Der Fettsud wird homogenisiert durch mehrmaliges Walzen auf einem Dreiwalzenstuhl. Diesem Homogeni¬ sierungsvorgang kommt besondere Bedeutung für das Geräuschverhalten zu. Man erhält auf diese Weise ein Fett der NLGI-Klasse 0 nach DIN ISO 2137. Dieses so erhaltene Fett wird auf einem Geräusch¬ prüfstand, welcher nach drei Frequenzbändern sowie nach maximalen Peaks differenziert, geprüft.The fat is homogenized by repeated rolling on a three-roll mill. This homogenization process is of particular importance for the noise behavior. In this way, a grease of NLGI class 0 according to DIN ISO 2137 is obtained. This fat obtained in this way is tested on a noise test bench, which differentiates according to three frequency bands and maximum peaks.
Gegenüber einem handelsüblichen Schmierfett aus ei¬ nem Mineralöl und einer langkettigen, verzweigten Polyharnstoffverbindung wurde eine deutliche Geräusch¬ verminderung gemessen.Compared to a commercially available lubricating grease made from a mineral oil and a long-chain, branched polyurea compound, a significant reduction in noise was measured.
Beispiel 2;Example 2;
In 839,5 g eines Esteröles, bestehend aus einem Ester der Trimellithsäure und einem Alkoholgemisch ausIn 839.5 g of an ester oil consisting of an ester of trimellitic acid and an alcohol mixture
Cg und C, «-Alkoholen, werden 74,5 g Diphenylmethan- diisocyanatCg and C, «alcohols, 74.5 g of diphenylmethane diisocyanate
(A CH. n = 2, B = aromatisches Monoisocyanat)(A CH. N = 2, B = aromatic monoisocyanate)
mit 75,5 g Octylamin (R = n-Octyl) in gleicher Weise wie in Beipiel 1 umgesetzt, mit Zusätzen versehen und homogenisiert.reacted with 75.5 g of octylamine (R = n-octyl) in the same way as in Example 1, provided with additives and homogenized.
Man erhäl* auf diese Weise ein Fett der NLGI-Klasse 1 nach DIN ISO 2137.In this way, a grease of NLGI class 1 according to DIN ISO 2137 is obtained.
Das so erhaltene Fett wird wie in Beispiel 1 geprüft und eine deutliche Geräuschverminderung gegenüber dem handelsüblichen Schmie fett gefunden.The fat thus obtained is tested as in Example 1 and a significant noise reduction compared to the commercially available grease is found.
Beispiel 3:Example 3:
In 839,5 g eines Esteröles, bestehend aus einem Ester der Pyro ellithsäure und einem isomeren C-8-Alko- hol, werden Diisocyanat und Amin wie in Beispiel 2 umgesetzt. Umsetzung, Additivierung und Homogeni¬ sierung erfolgen in gleicher Weise wie in Beispiel 1.In 839.5 g of an ester oil consisting of an ester the pyro ellitic acid and an isomeric C-8 alcohol, diisocyanate and amine are reacted as in Example 2. Implementation, additives and homogenization take place in the same way as in Example 1.
Man erhält auf diese Weise ein Fett der NLGI-Klasse 1 nach DIN ISO 2137.In this way, a grease of NLGI class 1 according to DIN ISO 2137 is obtained.
Das so erhaltene Fett wird wie in Beispiel 1 geprüft und eine deutliche Geräuschverminderung gegenüber dem handelsüblichen Schmierfett gefunden. The grease obtained in this way is tested as in Example 1 and a clear reduction in noise is found compared to the commercially available grease.
Die zahlenmäßige Auswertung der Beispiele geht aus den beigefügten Zeichnungen und Tabellen hervor.The numerical evaluation of the examples can be seen from the attached drawings and tables.
Es bedeutenMean it
Fig. 1 - die graphische E rstellung desFig. 1 - the graphical creation of the
Geräuschverhaltens der Schmierstoffe der Beispiele 1 bis 3 in je 3 Frequenz¬ bereichen (1) mit maximalen Spitzen¬ werten (2) bzw. (3).Noise behavior of the lubricants of Examples 1 to 3 in 3 frequency ranges (1) with maximum peak values (2) or (3).
Fig. 2 - die graphische Darstellung des Geräusch¬ verhaltens eines Vergleichsschmierstoffs nach dem Stand der Technik in drei Frequenzbereichen (1), (2), sowie mit dem maximalen Spitzenwert (4).Fig. 2 - the graphical representation of the noise behavior of a comparative lubricant according to the prior art in three frequency ranges (1), (2) and with the maximum peak value (4).
Tabelle 1 - die zahlenmäßige statistische Auswertung der Schmierstoffgeräuschprüfung gemäß Fig. 1 für Beispiele 1 bis 3 undTable 1 - the numerical statistical evaluation of the lubricant noise test according to FIG. 1 for examples 1 to 3 and
Tabelle 2 - die gleiche Auswertung für das Vergleichsfett gemäß Fig. 2. Table 2 - the same evaluation for the comparison fat according to FIG. 2.

Claims

Patentansprüche Claims
Schmierfettzusammensetzung aus einem Grundöl und einem kleineren Anteil eines Verdickungsmittels auf Basis einer Polyharnstoffverbindung sowie üblichen Additiven, d a d u r c h g e k e n n ¬ z e i c h n e t, daß das Grundöl ein Ester einer aromatischen Di-, Tri-, oder Tetracarbonsäure mit einem oder mehreren C--C, „-Alkanolen und dasGrease composition from a base oil and a smaller proportion of a thickener based on a polyurea compound and conventional additives, characterized ¬ characterized in that the base oil is an ester of an aromatic di-, tri-, or tetracarboxylic acid with one or more C - C, "-alkanols and the
/ 1o/ 1o
Verdickungsmittel das Reaktionsprodukt einer Ver¬ bindung der allgemeinen FormelThickener is the reaction product of a compound of the general formula
A(B)n (I)A (B) n (I)
und einem A in der allgemeinen Formel H-N-R (II), wobei in den Formelnand an A in the general formula H-N-R (II), wherein in the formulas
A = C Lg-πA = C Lg-π
B = aromatischer Mono- oder Diisocyanatrest n _ 1 - 3B = aromatic mono- or diisocyanate residue n _ 1-3
R = Alkyl- oder Alkenylrest mit 8 bis 22-C-Atomen oder Arylrest mit 6 bis 10-C-AtomenR = alkyl or alkenyl radical with 8 to 22 carbon atoms or aryl radical with 6 to 10 carbon atoms
ist, und wobei das Gemisch aus Grundöl und Ver¬ dickungsmittel eine Konsistenz mit einer Pene¬ tration von 220 - 385, 0,1mm aufweist.and the mixture of base oil and thickener has a consistency with a penetration of 220-385, 0.1 mm.
2. Schmierfettzusammensetzung nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t, daß B in Formel I ein 2,4- und/oder 2,6 Toluylendi- isocyanatrest ist. 2. Lubricating grease composition according to claim 1, which also means that B in formula I is a 2,4- and / or 2,6 tolylene diisocyanate residue.
EP90908203A 1989-06-02 1990-05-30 Lubricating grease composition Expired - Lifetime EP0433405B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3918107 1989-06-02
DE3918107A DE3918107A1 (en) 1989-06-02 1989-06-02 LUBRICATING GREASE COMPOSITION

Publications (2)

Publication Number Publication Date
EP0433405A1 true EP0433405A1 (en) 1991-06-26
EP0433405B1 EP0433405B1 (en) 1993-08-04

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US (1) US6063743A (en)
EP (1) EP0433405B1 (en)
JP (1) JPH0745677B2 (en)
KR (1) KR930007894B1 (en)
AT (1) ATE92518T1 (en)
AU (1) AU627892B2 (en)
BG (1) BG60784B1 (en)
BR (1) BR9006784A (en)
CA (1) CA2033074C (en)
DE (1) DE3918107A1 (en)
DK (1) DK0433405T3 (en)
ES (2) ES2020147A6 (en)
FI (1) FI910504A0 (en)
HU (1) HU211182B (en)
NO (1) NO910365L (en)
RO (1) RO109670B1 (en)
RU (1) RU1836410C (en)
WO (1) WO1990015125A1 (en)

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JP3330755B2 (en) * 1994-10-17 2002-09-30 日本精工株式会社 Grease composition
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DE19730318C2 (en) * 1997-07-15 2002-04-04 Klueber Lubrication Grease composition, process for making the same and their use
GB9803367D0 (en) 1998-02-17 1998-04-15 Exxon Research Engineering Co Lubricating grease composition and preparation
US6417143B1 (en) * 1998-10-30 2002-07-09 Ntn Corporation Rolling bearings and greases for the same
JP4327929B2 (en) * 1999-03-03 2009-09-09 協同油脂株式会社 Manufacturing method of urea grease with excellent noise reduction
US6498130B2 (en) * 2000-07-11 2002-12-24 Exxonmobil Research And Engineering Company Lubricating grease composition and preparation
US6916768B2 (en) * 2003-02-20 2005-07-12 Chevron U.S.A. Inc. Low noise grease gelling agents
US8889604B2 (en) 2010-07-30 2014-11-18 Chevron U.S.A. Inc. Method of preparing greases
US9012384B2 (en) 2010-07-30 2015-04-21 Chevron U.S.A. Inc. Method of preparing greases
RU2476588C2 (en) * 2011-02-14 2013-02-27 Российская Федерация, От Имени Которой Выступает Министерство Промышленности И Торговли Российской Федерации Grease for high-speed radial-axial bearings for gyroscopes and synchronous gyromotors
DE102020112993A1 (en) 2020-05-13 2021-11-18 Klüber Lubrication München Se & Co. Kg Lithium complex hybrid grease
WO2022019198A1 (en) * 2020-07-22 2022-01-27 株式会社ジェイテクト Raw material for grease, grease raw material production method, grease production method, and grease

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Also Published As

Publication number Publication date
HUT57823A (en) 1991-12-30
ATE92518T1 (en) 1993-08-15
KR930007894B1 (en) 1993-08-21
KR920701405A (en) 1992-08-11
EP0433405B1 (en) 1993-08-04
BR9006784A (en) 1991-08-06
AU627892B2 (en) 1992-09-03
BG60784B1 (en) 1996-03-29
ES2020147A6 (en) 1991-07-16
DE3918107A1 (en) 1990-12-06
JPH0745677B2 (en) 1995-05-17
JPH03504397A (en) 1991-09-26
ES2044594T3 (en) 1994-01-01
US6063743A (en) 2000-05-16
HU904230D0 (en) 1991-07-29
CA2033074A1 (en) 1990-12-03
RU1836410C (en) 1993-08-23
DK0433405T3 (en) 1993-12-27
BG93644A (en) 1993-12-24
RO109670B1 (en) 1995-04-28
WO1990015125A1 (en) 1990-12-13
AU5723290A (en) 1991-01-07
CA2033074C (en) 1994-02-15
HU211182B (en) 1995-11-28
NO910365D0 (en) 1991-01-31
FI910504A0 (en) 1991-02-01
NO910365L (en) 1991-01-31

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