EP1265976B1 - Composition lubrifiante comportant un agent dispersant, un compose de molybdene trinucleaire et un autre antioxydant different - Google Patents

Composition lubrifiante comportant un agent dispersant, un compose de molybdene trinucleaire et un autre antioxydant different Download PDF

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Publication number
EP1265976B1
EP1265976B1 EP01920802A EP01920802A EP1265976B1 EP 1265976 B1 EP1265976 B1 EP 1265976B1 EP 01920802 A EP01920802 A EP 01920802A EP 01920802 A EP01920802 A EP 01920802A EP 1265976 B1 EP1265976 B1 EP 1265976B1
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Prior art keywords
compound
composition
antioxidant
aminic
phenolic
Prior art date
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EP01920802A
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German (de)
English (en)
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EP1265976A1 (fr
Inventor
Jason Zhisheng Gao
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ExxonMobil Technology and Engineering Co
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ExxonMobil Research and Engineering Co
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    • 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
    • C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
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    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/04—Hydroxy compounds
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    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
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    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
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    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/09—Complexes with metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/02—Viscosity; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02—Pour-point; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/04—Detergent property or dispersant property
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/04—Detergent property or dispersant property
    • C10N2030/041—Soot induced viscosity control
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/40—Low content or no content compositions
    • C10N2030/41—Chlorine free or low chlorine content compositions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C10N2040/252—Diesel engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C10N2040/252—Diesel engines
    • C10N2040/253—Small diesel engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • C10N2070/02—Concentrating of additives

Definitions

  • This invention relates to a method of controlling the soot induced viscosity of diesel engine lubricant compositions.
  • soot Internal combustion engines usually function by the combustion of fuels which in turn generate the power needed to propel vehicles.
  • the fuel is a diesel fuel and the combustion thereof generally results in emissions from the exhausts of such vehicles which comprise three main components. These are: soot, particulate matter and nitrogen oxides (the latter will hereafter be abbreviated as NOx for convenience).
  • NOx nitrogen oxides
  • soot is generally formed as a result of incomplete combustion of the fuel. Soot adversely affects the performance of lubricants by increasing their viscosity (by accumulation of soot in the lubricant) and by causing wear.
  • soot does not increase the viscosity of the lubricant to undesirably high levels for it is also important to maintain the viscosity within the normal grades in order to enable quick and clean drainage of the engine during servicing.
  • the formation of soot may be alleviated to a significant extent by operating the diesel engine at relatively higher temperatures. However, the higher temperatures whilst mitigating the formation of soot also result in the formation of increased amounts of NOx. If, however, the engine temperature is lowered, incomplete combustion ensues and whilst this reduces the amount of NOx formed in the emissions, it also substantially increases the amount of soot generated.
  • the soot so formed can manifest itself in two ways.
  • soot can either appear as a thick black smoke emitted from the exhaust of the vehicle or can be accumulated in the engine lubricant.
  • soot builds up in the lubricant, the latter becomes more and more viscous and upon reaching a critical value can cause gelation of the lubricant and may eventually cause seizure of the engine.
  • Several methods have been tried to alleviate this problem including the use of one or more of dispersants, metal salts and solvents which may be ethers, esters and the like.
  • the dispersants function by forming a coating of the dispersant on the surface of soot particles and thereby minimising the tendency of the soot particles to agglomerate.
  • the potency of the dispersants to perform this function declines with time and thus, one of the methods of improving the useful life of lubricants, particularly crankcase lubricants, would be to improve the dispersancy retention capability of crankcase lubricants. This may be achieved, eg by minimising the risk of oxidation of the dispersants under the conditions prevalent in the engines during use.
  • the object of the present invention is to devise a method of mitigating the problem of soot induced viscosity increase in diesel lubricants by maximising the period for which the soot remains in the lubricant in a well dispersed state thereby controlling the rise in the absolute viscosity of the lubricant within the desired ranges for as long as is possible, ie minimising the increase in soot induced viscosity of the lubricant for longer than has been possible hitherto.
  • the object of the present invention is to improve the dispersancy retention capability of such lubricants.
  • the present invention comprises diesel engine lubricant composition
  • a base stock comprising a dispersant and an antioxidant comprising an oil soluble trinuclear organomolybdenum compound of the generic formula: Mo 3 S x -(Q) wherein x is from 4 to 10, preferably 7, and Q is a core group, which may be a ligand, and at least one other compound selected from a phenolic and an aminic compound.
  • compositions of the present invention are those that comprise a major amount of a lubricating oil as base stock suitable for use in an engine crankcase, particularly a diesel engine crankcase.
  • a lubricating oil as base stock suitable for use in an engine crankcase, particularly a diesel engine crankcase.
  • natural or synthetic lubricating oils having a kinematic viscosity of 3.5 to 25 mm 2 /s (cSt) at 100°C comprise a major portion of the lubricating compositions.
  • the dispersancy retention properties of such lubricant compositions is improved in accord with this invention by including in the crankcase lubricant an added oil soluble organomolybdenum compound and at least one other compound selected from a phenolic and an aminic compound.
  • the trinuclear molybdenum compounds are of formula (I) Mo 3 S x -(Q) wherein x is from 4 to 10, preferably 7, and Q is a core group are relatively new and are claimed and described in our prior published US-A-5,906,968. The matter disclosed in this prior US patent on the structure, preparation and properties of the trinuclear molybdenum compounds is incorporated herein by reference.
  • the core group (Q) may be a ligand capable of rendering the organomolybdenum compound of formula (I) oil soluble and ensuring that said molybdenum compound is substantially charge neutral.
  • the core group (Q) is generally associated with suitable ligands such as L y wherein L is the ligand and y is of a sufficient number, type and charge to render the compound of formula (I) oil soluble and to neutralise the charge on the compound of formula (I) as a whole.
  • suitable ligands such as L y wherein L is the ligand and y is of a sufficient number, type and charge to render the compound of formula (I) oil soluble and to neutralise the charge on the compound of formula (I) as a whole.
  • the trinuclear molybdenum compound used in the compositions of the present invention may be represented by the formula (II): Mo 3 S x L y
  • the ligands "L” are suitably dihydrocarbyl dithiocarbamates of the structure (-S 2 CNR 2 ) wherein the dihydrocarbyl groups, R 2 impart oil solubility to the molybdenum compound.
  • hydrocarbyl denotes
  • the hydrocarbyl groups are preferably alkyl (e.g, in which the carbon atom attached to the remainder of the ligand "L" is primary, secondary or tertiary), aryl, substituted aryl and/or ether groups.
  • the hydrocarbyl groups of the ligands should be such that they have a sufficient number of carbon atoms to render the compound (I) soluble or dispersible in the oil to which the trinuclear organomolybdenum compound containing the ligand is added.
  • the total number of carbon atoms present among all of the hydrocarbyl groups of the organomolybdenum compounds' ligands is suitably at least 21, preferably at least 25, more preferably at least 30 and even more preferably at least 35, typically e.g., 21 to 800.
  • the number of carbon atoms in each hydrocarbyl group will generally range from 1 to 100, preferably from 1 to 40 and more preferably from 3 to 20.
  • the antioxidant in the compositions of the present invention include at least one other compound selected from a phenolic compound and an aminic compound.
  • phenolic compounds hindered phenols are preferred.
  • phenolic compounds include inter alia :
  • Suitable aminic compounds for use in the compositions of the present invention are diaryl amines, aryl naphthyl amines and alkyl derivatives of diaryl amines and the aryl naphthyl amines.
  • Preferred aminic antioxidants are represented by the formulae (VII) and (VIII) wherein each of R 4 and R 5 is a hydrogen atom or represents the same or different alkyl groups from 1-8 carbon atoms.
  • Monoalkyldiphenyl amines such as eg monooctyldiphenyl amine and monononyl diphenyl amine; dialkyldiphenyl amines such as eg 4,4'-dibutyldiphenyl amine, 4,4'-dipentyldiphenyl amine, 4,4'-dihexyldiphenyl amine, 4,4'-diheptyldiphenyl amine, 4,4'-dioctyldiphenyl amine and 4,4'-dinonyldiphenyl amine; polyalkyldiphenyl amines such as eg tetra-butyldiphenyl amine, tetra-hexyldiphenyl amine, tetra-octyldiphenyl amine and tetranonyldiphenyl amine; the naphthylamines such as eg ⁇ -naphthy
  • the antioxidant which comprises the organomolybdenum compound in combination with a phenolic and/or an aminic compound will form a minor component of the total lubricant composition.
  • the organomolybdenum compound typically will comprise 0.05 to 5.00 wt % of the total composition, preferably from 0.05 to 2.0 wt%, and more preferably from 0.1 to 0.7 wt%, i.e., the molybdenum metal is suitably present in an amount of from 25 to 2500 ppm, preferably from 50 to 1000 ppm, and more preferably from 100 to 700 ppm, and the phenolic and/or aminic compounds 0.10 to 3.0 wt % of the total composition.
  • the antioxidant comprises in addition to the organo molybdenum compound a mixture of the phenols (III) and (IV) above and the diaryl amine (V) in a weight ratio ranging from 80:10:10 to 40:20:40 respectively, preferably typically 75:15:15 respectively.
  • the antioxidants may be combined with a carrier liquid in the form of a concentrate.
  • concentration of the combined antioxidants in the concentrate may vary from 1 to 80% by weight, and will preferably be in the range of 5 to 10% by weight.
  • the antioxidant combination of the present invention can be used with any of the conventional dispersants used hitherto in the lubricating compositions.
  • dispersants include inter alia the polyalkylene succinimides, Mannich condensation products of polylalkylphenol-formaldehyde polyamine and boronated derivatives thereof.
  • ashless dispersants such as the ashless succinimides, especially the polyisobutenyl succinimides of a polyamine such as eg tetraethylenepentamine or its homologues, benzylamine ashless dispersants, and ester ashless dispersants.
  • the dispersants are generally used in the compositions of the present invention in an amount ranging from 2-10% by weight based on the total weight of the lubricant composition, preferably from 4-8% by weight.
  • these lubricating compositions may include additives commonly used in lubricating oils especially crankcase lubricants, such as antiwear agents, detergents, rust inhibitors, viscosity index improvers, extreme-pressure agents, friction modifiers, corrosion inhibitors, emulsifying aids, pour point depressants, anti-foams and the like.
  • crankcase lubricants such as antiwear agents, detergents, rust inhibitors, viscosity index improvers, extreme-pressure agents, friction modifiers, corrosion inhibitors, emulsifying aids, pour point depressants, anti-foams and the like.
  • a feature of the lubricant compositions of the present invention is that the presence therein of trinuclear organomolybdenum compounds in combination with a phenolic and/or an aminic compound as antioxidant provides unexpected improvement in oxidation control, viscosity increase control and dispersancy retention over compositions which contain only one of these antioxidants used alone.
  • Test oils were prepared. These oils were then tested in a bench oxidation test which was conducted at 165°C under a mixed nitrogen/air flow, with 40 ppm iron from added ferric acetylacetonate as catalyst. The flow rates of air and nitrogen were controlled at 500 ml/min and 350ml/min respectively.
  • the remaining dispersancy of the Test oil after 32 hours in the bench oxidation test was then determined by use of a GM 6.2L soot-laden basestock dispersancy test in which the soot dispersancy of an used oil was determined by viscosity ratio of the diluted Test oil in the presence and absence of soot; the lower the ratio, the better the dispersancy.
  • the Test oil was mixed with a soot-laden 600 SN basestock (3.5-4.5% by weight soot) from the GM 6.2L engine at the ratio of 25:75 by weight and the kinematic viscosity at 100°C of the Test oil and fresh base oil (soot-free 600SN) mixture at the same ratio (25:75) was also measured.
  • Fresh oil dispersancy was also determined using the same method.
  • Test Oils A-E are shown in Table 1 below: Test Oils A B C D E 600 SN (% wt) 94.0 93.0 93.0 93.0 93.0 Paranox® 106 (% wt) 6.0 6.0 6.0 6.0 6.0 Irganox® L150 - 1.0 - 0.5 0.5 Mo 3 -dithiocarbamate - - 1.0 0.5 - Molyvan® 822 (% wt) - - - - 0.5
  • Table 3 shows the characteristics of the used oils (A-E) after the oxidation test.
  • compositions of the Test oils used in Examples (F-R) are shown in Table 4 below:

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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 (10)

  1. Procédé de réglage de la viscosité, induite par la suie, d'une composition lubrifiante pour moteur Diesel, comprenant une huile de base et un agent dispersant en ajoutant une quantité efficace d'un antioxydant, caractérisé en ce que l'antioxydant comprend un composé d'organomolybdène trinucléaire soluble dans l'huile de formule générale : Mo3Sx-(Q) dans laquelle x est 4 à 10 et Q est un groupe central, qui peut être un ligand, et au moins un autre composé choisi parmi un composé phénolique et un composé aminé.
  2. Procédé selon la revendication 1, dans lequel ladite composition comprend une quantité majeure d'une huile lubrifiante naturelle ou synthétique ayant une viscosité cinématique de 3,5 à 25 mm2/s (cSt) à 100°C.
  3. Procédé selon l'une quelconque des revendications précédentes, dans lequel les composés d'organomolybdène trinucléaires ont pour formule (I) : Mo3Sx-(Q) dans laquelle x est 7 et Q est un groupe central.
  4. Procédé selon l'une quelconque des revendications précédentes, dans lequel le groupe central Q est un ligand capable de rendre le composé d'organomolybdène de formule (I) soluble dans l'huile et de garantir que ledit composé de molybdène est sensiblement de charge neutre.
  5. Procédé selon l'une quelconque des revendications précédentes, dans lequel le composé phénolique est un phénol empêché.
  6. Procédé selon l'une quelconque des revendications précédentes, dans lequel le composé aminé est choisi parmi un ou plusieurs des diarylamines, des arylnaphtylamines et des dérivés alkyliques de diarylamines et d'arylnaphtylamines de formule (VII) ou (VIII) données ci-dessous, dans lesquelles chacun de R4 et R5 est un atome d'hydrogène ou représente des groupes alkyle identiques ou différents de 1 à 8 atomes de carbone :
    Figure 00190001
    Figure 00190002
  7. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'antioxydant, qui comprend le composé d'organomolybdène trinucléaire et au moins un autre composé choisi parmi un composé phénolique et/ou aminé, forme un composant mineur de la composition lubrifiante totale.
  8. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'antioxydant, qui comprend le composé d'organomolybdène trinucléaire et un composé aminé, forme un composant mineur de la composition lubrifiante totale.
  9. Procédé selon l'une quelconque des revendications précédentes, dans lequel le composé d'organomolybdène trinucléaire est présent dans ladite composition en quantité de 0,05 à 5,00 % en poids de la composition totale.
  10. Procédé selon l'une quelconque des revendications précédentes, dans lequel la quantité de composés phénoliques et/ou aminés présents dans ladite composition est de 0,10 à 3,0 % en poids de la composition totale.
EP01920802A 2000-02-14 2001-02-08 Composition lubrifiante comportant un agent dispersant, un compose de molybdene trinucleaire et un autre antioxydant different Expired - Lifetime EP1265976B1 (fr)

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US8383563B2 (en) 2007-08-10 2013-02-26 Exxonmobil Research And Engineering Company Method for enhancing the oxidation and nitration resistance of natural gas engine oil compositions and such compositions

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EP1323816A1 (fr) * 2001-12-21 2003-07-02 Infineum International Limited Compositions d'huiles lubrifiantes pour moteur diesel de grande puissance
EP1321507A1 (fr) * 2001-12-21 2003-06-25 Infineum International Limited Compositions d'huiles lubrifiantes pour moteur diesel de grande puissance
CN114644951A (zh) * 2021-03-25 2022-06-21 上海济唐润滑材料科技有限公司 一种汽车发动机润滑油及其应用

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US6010987A (en) * 1996-12-13 2000-01-04 Exxon Research And Engineering Co. Enhancement of frictional retention properties in a lubricating composition containing a molybdenum sulfide additive in low concentration
WO1998026030A1 (fr) * 1996-12-13 1998-06-18 Exxon Research And Engineering Company Compositions d'huile lubrifiante contenant des complexes de molybdene organiques
US5837657A (en) * 1997-12-02 1998-11-17 Fang; Howard L. Method for reducing viscosity increase in sooted diesel oils
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US8383563B2 (en) 2007-08-10 2013-02-26 Exxonmobil Research And Engineering Company Method for enhancing the oxidation and nitration resistance of natural gas engine oil compositions and such compositions

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JP2003523455A (ja) 2003-08-05
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