EP0280579B1 - Lubrifiants ayant une teneur basse en phosphore et zinc - Google Patents

Lubrifiants ayant une teneur basse en phosphore et zinc Download PDF

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Publication number
EP0280579B1
EP0280579B1 EP88301711A EP88301711A EP0280579B1 EP 0280579 B1 EP0280579 B1 EP 0280579B1 EP 88301711 A EP88301711 A EP 88301711A EP 88301711 A EP88301711 A EP 88301711A EP 0280579 B1 EP0280579 B1 EP 0280579B1
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EP
European Patent Office
Prior art keywords
composition
oil
copper
sulphur
phosphorus
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
EP88301711A
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German (de)
English (en)
Other versions
EP0280579A2 (fr
EP0280579A3 (en
Inventor
Terence Colclough
John Frederick Marsh
Frederick Alastair Gibson
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ExxonMobil Chemical Patents Inc
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Exxon Chemical Patents Inc
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Priority to AT88301711T priority Critical patent/ATE82316T1/de
Publication of EP0280579A2 publication Critical patent/EP0280579A2/fr
Publication of EP0280579A3 publication Critical patent/EP0280579A3/en
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Publication of EP0280579B1 publication Critical patent/EP0280579B1/fr
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/08—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic sulfur-, selenium- or tellurium-containing compound
    • 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
    • C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
    • 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
    • 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
    • C10M129/10—Hydroxy compounds having hydroxy groups bound to a carbon atom of a six-membered aromatic ring
    • 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
    • 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
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
    • 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
    • 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
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
    • C10M129/42—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms polycarboxylic
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/56—Acids of unknown or incompletely defined constitution
    • C10M129/58—Naphthenic acids
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    • C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/52—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of 30 or more atoms
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/02—Sulfurised compounds
    • C10M135/04—Hydrocarbons
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    • C10M135/02—Sulfurised compounds
    • C10M135/06—Esters, e.g. fats
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
    • C10M135/18—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond thiocarbamic type, e.g. containing the groups
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/20—Thiols; Sulfides; Polysulfides
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/20—Thiols; Sulfides; Polysulfides
    • C10M135/28—Thiols; Sulfides; Polysulfides containing sulfur atoms bound to a carbon atom of a six-membered aromatic ring
    • C10M135/30—Thiols; Sulfides; Polysulfides containing sulfur atoms bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/32—Heterocyclic sulfur, selenium or tellurium compounds
    • C10M135/36—Heterocyclic sulfur, selenium or tellurium compounds the ring containing sulfur and carbon with nitrogen or oxygen
    • C—CHEMISTRY; METALLURGY
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    • C10M139/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
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    • C10M141/12—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic compound containing atoms of elements not provided for in groups C10M141/02 - C10M141/10
    • C—CHEMISTRY; METALLURGY
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    • C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/10—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate
    • C10M145/12—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate monocarboxylic
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    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10M145/16—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate polycarboxylic
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    • C10M149/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M149/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amino group
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    • C10M149/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M149/10—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a nitrogen-containing hetero ring
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    • C10M149/14—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds a condensation reaction being involved
    • C10M149/22—Polyamines
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    • C10M159/24—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products containing sulfonic radicals
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    • C10N2040/251—Alcohol fueled engines
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    • C10N2040/255—Gasoline engines
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    • C10N2040/25—Internal-combustion engines
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    • C10N2040/28—Rotary engines
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    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • C10N2070/02—Concentrating of additives

Definitions

  • the present invention relates to lubricating compositions, especially automobile crankcase lubricants, containing low or zero amounts of phosphorus and zinc.
  • This invention provides lubricant compositions and concentrates with low or zero amounts of phosphorus and zinc, and which comprise copper, sulphur, and a bearing corrosion inhibitor, which compositions have been found to have remarkable engine performance.
  • US-A-2356661 deals with lubricating oils containing 50 to 1000 parts per million of copper as an oil-soluble organic compound such as copper dialkyl dithiocarbamates and including phosphorus containing compounds together with from 0.1 to 0.5 wt % of total sulphur in the oil, sulphur being provided as oil-soluble organic sulphur compounds such as thiocarbamates.
  • US-A-2343756 discloses the addition of copper compounds including phosphorus-containing copper complexes in conjunction with sulphur compounds, to lubricating oils. Amounts of from 0.1 to 0.5 wt % of sulphur are disclosed, with amounts in excess of 0.5 wt % sulphur described as being potentially detrimental.
  • cuprous thiophosphates are included in lubricant compositions at relatively high levels, which will give high phosphorus level in the oils.
  • US-A-3346493 a wide variety of metal-containing polymeric amine-metal reactants are employed as detergents in lubricant compositions.
  • a lubricant containing inter alia, a copper salt of an acylated nitrogen compound, 0.075% phosphorus as a ZDDP reacted with hexene oxide, and a sulphurized methyl ester of a tall oil acid.
  • Other copper containing lubricants either contain more phosphorus or no sulphur.
  • US-A-4122033 discloses the entire group of transition metal compounds as antioxidation stabilizers in conjunction with amines, selenides, phosphines or phosphites and may be used in various applications including as additives for lubricants. None of the foregoing documents describe fully formulated lubricant oils which would be appropriate to meet the requirements for modern lubricants and none specifically address the reduction of phosphorus levels while maintaining performance in antiwear, antioxidation and corrosion inhibition.
  • EP-A-24146 discloses lubricant compositions containing an ashless dispersant and/or polymeric viscosity index improver dispersant and copper which may be in the form of a dithiocarbamate, but requires the presence of from 0.01 to 0.5 wt% zinc and from 0.01 to 0.5 wt % phosphorus.
  • Thiadiazole polysulphides are an optional component.
  • US-A-4330420 describes oils with reduced phosphorus content (but only to 0.05%P) using mixtures of dialkyldiphenylamine and a sulphurized polyolefin to compensate for reduction in the amount of ZDDP. There is no disclosure of the use of copper or thiadiazole polysulphides.
  • EP-A-89844 describes reaction products of 4,4 ⁇ -methylene-(2,6-di-t-butyl phenol) and tri-Sec-C4 ⁇ 12 alkyl orthoborate and their use in lubricants to enable the amount of ZDDP to be reduced to provide from 0.05 to 0.11 wt % p.
  • US-A-4490265 describes lubricating oils comprising boron-containing heterocyclic compounds which may be in the form of a metal salt including a copper salt, thiadiazole polysulphides, terephthalic acid and as an oxidation inhibitor either a bis(dithiobenzil) metal derivative where the metal may inter alia be copper or a sulphur-bridged, bis hindered phenol.
  • a bis(dithiobenzil) metal derivative where the metal may inter alia be copper or a sulphur-bridged, bis hindered phenol.
  • the desirability of reducing or eliminating phosphorus is not disclosed and all the Examples of lubricants contain 0.05 wt% P.
  • US-A-4623474 contains a similar disclosure.
  • US-A-4627930 also describes boron-containing heterocyclic compounds which may be in the form of a copper salt and may be sulphurized.
  • Thiadiazole polysulphides and copper carboxylates are also disclosed.
  • the boron-containing heterocyclic compounds are described as phosphorus-free, there is no disclosure of a fully formulated oil containing less than 0.05 wt % P.
  • US-A-4 629 580 contains a similar disclosure, as does US-A-4 595 514.
  • US-A-4 629 579 discloses boron and metal-boron derivatives for use as extreme pressure, anti-wear and friction reducing additives for lubricating oils and compositions including one containing no ZDDP, but there is disclosure of a composition containing low or zero amounts of phosphorus, with sulphur and copper.
  • GB-A-779825 discloses an antioxidant for hydrocarbon oils, the antioxidant comprising a copper compound and a relatively small amount (0.4 % in the Examples) of an iron, nickel or cobalt derivature of an alkyldithio acid or acids.
  • WO-A-8707291 relates to the use of low concentrations of an oil-soluble transition metal compound for ameliorating low temperature thickening in automatic transmission fluids and high temperature thickening in gear lubricants, copper compounds being mentioned in this context.
  • Lubricant compositions which exhibit improved resistance to high temperature thickening and a dramatic reduction in the formation of insoluble resins are disclosed.
  • compositions disclosed therein may contain a dithiocarbamate of any monovalent or polyvalent metal and lists the alkaline earth metals, zinc, cadmium, magnesium, tin, molybdenum, iron, copper, nickel, cobalt, chromium and lead as examples of suitable polyvalent metals, the Group II metals being preferred.
  • compositions may contain ZDDPs, and indicates a low level of phosphorus as being less than 0.1%.
  • the invention seeks to provide lubricants having antiwear, corrosion inhibition and antioxidant performance appropriate to modern oil requirements with reduced or zero amounts of zinc and phosphorus and without the need for large amounts and/or expensive forms of antioxidant.
  • Lubricants with reduced or zero amounts of phosphorus are disclosed and claimed in European Application No. 88.301 712.1.
  • modern oil as used herein in relation to automobile crankcase lubricants refers to oil which can meet the current requirements for crankcase lubricants in the major industrial countries.
  • This invention is particularly concerned with automobile lubricants which can meet and exceed the requirements for the SF API Engine Service Category for service station oils and/or the CD requirements for the CD/API Engine Service Category for Commercial Oils (Diesel Engines) established jointly by API, SAE and ASTM.
  • this invention provides a lubricant composition
  • a lubricant composition comprising a major amount of a lubricating oil, 5 to 500 parts per million by weight (ppm) of added copper present in oil-soluble form, one or more added oil-soluble sulphur-containing compounds such that the composition preferably comprises from greater than 0.5 to 2.0 wt % of total sulphur, more preferably 0.5 to 1.0 wt % of total sulphur, and an effective amount of a bearing corrosion inhibitor, the composition containing less than 0.05 wt % phosphorus and less than 0.01 wt% zinc, preferably being substantially phosphorus-free and zinc-free.
  • the lubricant composition will also contain one or more ashless dispersants and/or one or more viscosity index improver dispersants and/or one or more overbased additives which function as antacid and anti-rust agents, such as overbased calcium or magnesium sulphonates or phenates.
  • the use of copper in the invention enables a low phosphorus oil with performance meeting the requirements for modern oils to be obtained economically and with good control of oxidation, which in an automobile engine is catalysed by metal accumulated in the oil by wear or corrosion, with iron being a particular oxidation catalyst.
  • the anti-oxidant effect may not be sufficient for some applications.
  • the ash level of the oil will be increased and an increased tendency to bearing corrosion may be observed.
  • the amount of added copper in the compositions will generally be within the range of 10 to 400 ppm, typically 10 to 300 ppm, preferably 10 to 200 ppm, e.g. 60 to 200 ppm.
  • compositions of the invention comprising low amounts of oil-soluble copper compounds and very low or zero amounts of phosphorus to provide adequate antioxidant and antiwear performance for the stringent requirements of modern engine tests is surprising. Copper is known to act in many situations as an oxidation promoter or catalyst, and closely related metals, such as cobalt and chromium, are not effective lubricant anti-oxidants.
  • EP-A-24146 teaches the presence of at least 0.01 wt % of each of phosphorus and zinc.
  • the copper compound functions effectively in compositions which may contain zinc and other metal compounds, such as calcium or magnesium overbased additives, which have an inherent pro-oxidant activity.
  • the copper compounds used as anti-oxidants in this invention may be chosen from those described in EP-A-24146 as suitable for lubricants provided that the copper compounds are substantially free of phosphorus.
  • the copper may be blended into the oil as the oil soluble copper salt of a synthetic or natural carboxylic acid.
  • suitable carboxylic acids include C10 to C18 fatty acids such as stearic or palmitic acid, unsaturated acids such as oleic acid, branched carboxylic acids such as naphthenic acids of molecular weight from 200 to 500, neodecanoic or 2-ethylhexanoic acid and alkyl or alkenyl substituted dicarboxylic acids such as polyalkene substituted succinic acids, e.g. octadecenyl succinic acids, dodecenyl succinic acids and polyisobutenyl succinic acids.
  • the copper may be blended into the oil as oil-soluble copper dithiocarbamates of the general formula (RR ⁇ NCSS) n Cu, where n is 1 or 2 and R and R ⁇ are the same or different hydrocarbyl radicals containing 1 to 18, preferably 2 to 12 carbon atoms such as alkyl, alkenyl, aryl, aralkyl, alkaryl and cycloalkyl radicals.
  • R and R ⁇ are the same or different hydrocarbyl radicals containing 1 to 18, preferably 2 to 12 carbon atoms such as alkyl, alkenyl, aryl, aralkyl, alkaryl and cycloalkyl radicals.
  • Other copper and sulphur containing compounds such as copper mercaptides, disulphides and thioxanthates are suitable for use in the invention. Copper sulphonates, phenates, and acetylacetonates may also be used.
  • the copper may be introduced in the oil in an oil-insoluble form provided that in the finished lubricant composition the copper is in the form on an oil-soluble compound.
  • the term "added copper” is intended to exclude copper present in the oil as a result of accumulation of copper in the oil during use, e.g. by wear or corrosion of copper-containing components.
  • the lubricant compositions of the invention contain an added oil-soluble sulphur compound.
  • sulphur compounds are the dithiocarbamates, preferably of the formula: (RR ⁇ NCSS) n M, wherein R, R ⁇ and n are as defined hereinbefore and M is a suitable metal such as molybdenum or (as indicated above) copper or a optionally substituted hydrocarbyl radical.
  • Preferred dithiocarbamates are dialkyl dithiocarbamates preferably containing 2 to 12 carbon atoms such as diamyl dithiocarbamates.
  • Sulphur may also be introduced as a mercaptide particularly the mercaptides of aliphatic mercaptans (including copper mercaptides as indicated above), sulphurized unsaturated organic compounds including sulphurized olefins (e.g. US-A-4119549, US-A-4119550, US-A-4191659 and US-A-4147640), sulphurized Diels-Alder adducts (e.g.
  • Mineral lubricating oils contain sulphur, whereas synthetic oils may be sulphur-free, so that the amount of sulphur added as a sulphur-containing compound varies according to the basestock and the sulphur contents of other components in the lubricating composition, more preferably so as to give a sulphur content of greater than 0.5 to 1.0 wt % total sulphur.
  • the lubricant compositions of the invention advantageously contain from 0.5 to 0.7 wt % total S, and most preferably 0.1 to 0.5 wt % S as added oil-soluble sulphur-containing compound preferably in the form of a sulphurized ester.
  • the bearing corrosion inhibitor is a corrosion inhibitor effective at inhibiting corrosion effects on bearings such as Cu/Pb bearings, where effects such as copper staining and high weight loss can be encountered. Such additives have been found to promote the anti-wear performance of the oil.
  • Preferred bearing corrosion inhibitors are borate esters such as B(OR)3, (RO)2B-O-B(OR)2 or (ROBO)3, (RO)2BOR1OB(OR)2 and mixtures (wherein R is a substituted or unsubstituted alkyl, aryl or aralkyl group or two groups R together form a substituted or unsubstituted alkylene group and R1 is a substituted or unsubstituted alkylene group) and these materials may be derived, for example, from alcohols such as alkoxyalkanols (both short chain alkanols and longer chain alcohols as in US-A-4440656) and polyetheralkanols; mono-,di- and trihydroxy alkanls
  • triethanolamine and tri-isopropanolamine hydroxyamines made by reacting a primary amine (e.g. oleylamine) or secondary amine with ethylene or propylene oxide and the compounds of US-A-4406802.
  • Preferred alcohols are 2-methylpentan-1,3-diol, butane-1,2-diol, butane-1,3-diol and similar 1,2 and 1,3 diols, and ethoxyethanol.
  • the invention contains from 0.01 to 10 wt %, preferably 0.1 to 5 wt %, of a borate ester especially an ester of an alkoxyalkanol or a polyetheralkanol, e.g. a tris(ethoxyethyl) orthoborate ester or metaborate ester, or a biborate of a diol such as butane-1,3-diol.
  • a borate ester especially an ester of an alkoxyalkanol or a polyetheralkanol, e.g. a tris(ethoxyethyl) orthoborate ester or metaborate ester, or a biborate of a diol such as butane-1,3-diol.
  • the bearing corrosion inhibitor is a thiadiazole mercaptan, especially a thiadiazole polysulphide containing from 5 to 50 carbon atoms, a derivative or polymer thereof.
  • Preferred materials are the derivatives of 1,3,4 thiadiazole polysulphides such as those described in US-A-2719125, 2719126 and 3087932.
  • the compound 2,5-bis (t-octadithio)-1,3,4-thiadiazole commercially available as Amoco 150 or 2,5-bis(nonyldithio)-1, 3,4-thiadiazole available as Amoco 158.
  • thiadiazole mercaptans may be used such as esters, condensation products with halogenated carboxylic acids, reaction products with aldehydes and amines, alcohols or mercaptans, amine salts, dithiocarbamates, reaction products with ashless dispersants (e.g. US-A-4140643 and US-A-4136043) and reaction products with sulphur halides and olefins.
  • These materials are preferably present in an amount of from 0.01 to 10 wt %, more preferably 0.1 to 5.0 wt % of the lubricant composition.
  • the lubricating compositions may comprise small amounts of phosphorus, less than 0.05 wt %, preferably less than 0.01 wt%, more preferably less than 0.005 wt %, but more preferably the lubricating compositions are substantially free of phosphorus.
  • the lubricating composition further comprises:
  • the nitrogen containing dispersant additives are those known in the art as sludge dispersants for crankcase motor oils, e.g. such as shown in US-A-3275554, US-A-3565804, US-A-3442808, US-A-3442808, GB-A-983040 or BE-A-658236.
  • dispersants are those formed by reacting alkenyl succinic anhydride, e.g. polyisobutenyl succinic anhydride, and an amine described in US-A-3202678, 3154560, 3172892, 3024195, 3024237, 3219666, 3216936 and BE-A-662875.
  • alkenyl succinic anhydride e.g. polyisobutenyl succinic anhydride
  • an amine described in US-A-3202678, 3154560, 3172892, 3024195, 3024237, 3219666, 3216936 and BE-A-662875.
  • the ashless dispersants may be esters derived from long chain hydrocarbon substituted carboxylic acids and from hydroxy compounds such as monohydric and polyhydric alcohols or aromatic compounds such as phenols and naphthols as prepared for example in US-A-3522179.
  • Hydroxyamines which can be reacted with any of the aforesaid long chain hydrocarbon substituted carboxylic acids to form dispersants include 2-amino-1-butanol, 2-amino-2-methyl-1-propanol, p-(beta-hydroxyethyl)-aniline, 2-amino-1-propanol, 3-amino-1-propanol, 2-amino-2-methyl-1 3-propane-diol, 2-amino-2-ethyl-1, 3-propanediol, N-(beta-hydroxy-propyl)-N ⁇ -(beta-aminoethyl)-piperazine, tris(hydroxmethyl) amino-methane (also known as trismethylolaminomethane), 2-amino-1-butanol, ethanolamine, beta-(beta-hydroxyethoxy)-ethylamine, and the like. Mixtures of these or similar amines can also be employed.
  • Preferred dispersants are those derived from polyisobutenyl succinic anhydride and polyethylene amines, e.g. tetraethylene pentamine, polyoxyethylene and polyoxypropylene amines, e.g. polyoxypropylene diamine, trismethylolaminomethane and pentaerythritol, and combinations thereof.
  • One particularly preferred dispersant combination involves a combination of (A) polyisobutenyl succinic anhydride with (B) a hydroxy compound, e.g. pentaerythritol, (C) a polyoxyalkylene polyamine, e.g. polyoxypropylene diamine, and (D) a polyalkylene polyamine, e.g.
  • polyethylene diamine and tetraethylene pentamine using about 0.01 to about 4 equivalents of (B) and (D) and about 0.01 to about 2 equivalents of (C) per equivalent of (A) as described in US-A-3894763.
  • Another preferred dispersant combination involves the combination of (A) polyisobutenyl succinic anhydride with (B) a polyalkylene polyamine, e.g. tetraethylene pentamine, and (C) a polyhydric alcohol or polyhydroxy-substituted aliphatic primary amine, e.g. pentaerythritol or trismethylolaminomethane as described in US-A-3632511.
  • the alkenyl succinic polyamine type dispersants can be further modified with a boron compound such as boron oxide, boron halides, boron acids and ester of boron acids in an amount to provide 0.1 to 10 atomic proportions of boron per mole of the acylated nitrogen compound as generally taught in US-A-3087936 and 3254025. Mixtures of dispersants can also be used such as those described in US-A-4113639.
  • a boron compound such as boron oxide, boron halides, boron acids and ester of boron acids in an amount to provide 0.1 to 10 atomic proportions of boron per mole of the acylated nitrogen compound as generally taught in US-A-3087936 and 3254025.
  • Mixtures of dispersants can also be used such as those described in US-A-4113639.
  • the oils may contain from 1.0 to 10 wt %, more preferably 2.0 to 7.0 wt % of these dispersants.
  • the dispersancy may be provided by 0.3 to 10% of a polymeric Viscosity Index improver dispersant, for example copolymers of alkyl methacrylates with N-vinyl pyrrolidone or dimethylaminoalkyl methacrylate, alkyl fumarate-vinyl acetate N-vinyl pyrolidine copolymers, post-grafted interpolymers of ethylene-propylene with an active monomer such as maleic anhydride which may be further reacted with an alcohol or an alkylene polyamine, such as in US-A-4149984; or styrene/maleic anhydride polymers post-reacted with alcohols and amines, ethoxylated derivatives of acrylate polymers such as in US-A-3702300.
  • a polymeric Viscosity Index improver dispersant for example copolymers of alkyl methacrylates with N-vinyl pyrrolidone or dimethylaminoalky
  • Magnesium and/or calcium containing additives are frequently included in lubricating compositions either alone or in combination with other alkali metal or alkaline earth metal additives such as those containing sodium. These may be present for example as the metal salts of sulphonic acids, alkyl phenols, sulphurised alkyl phenols, alkyl salicylates, naphthenates, and other oil soluble mono- and di-carboxylic acids.
  • Highly basic alkaline earth metal alkaryl sulfonates are generally known for example in US-A-3150088 and 3150089.
  • a preferred alkaline earth sulfonate is magnesium alkyl aromatic sulfonate having a total base number (TBN, as measured by the procedure of ASTM D2896) ranging from 300 to 400.
  • Polyvalent metal alkyl salicylate and naphthenate materials may also be included, such as the methylene and sulfur bridged materials which are readily derived from alkyl substituted salicylic or naphthenic acids or mixtures of either or both with alkyl substituted phenols.
  • Basic sulfurized salicylates and a method for their preparation are shown in US-A-3595791.
  • the individual R groups may each contain from 5 to 40, preferably 8 to 20, carbon atoms.
  • the metal salt is prepared by reacting an alkyl phenol sulfide with a sufficient quantity of metal containing material to impart the desired alkalinity to the sulfurized metal phenate.
  • the sulfurized alkyl phenol is converted by reaction with a metal containing material including oxides, hydroxides and complexes in an amount sufficient to neutralize said phenol and, if desired, to overbase the product to a desired alkalinity by procedures well known in the art.
  • a metal containing material including oxides, hydroxides and complexes in an amount sufficient to neutralize said phenol and, if desired, to overbase the product to a desired alkalinity by procedures well known in the art.
  • Preferred is a process of neutralization utilizing a solution of metal in a glycol ether.
  • Magnesium and calcium containing additives such as described above although beneficial in other respects can increase the tendency of the lubricating oil to oxidise. This is especially true of the highly basic sulphonates.
  • the invention therefore provides a crankcase lubricating composition also containing from 2 to 8000 parts per million of calcium and/or magnesium.
  • the magnesium and/or calcium is generally present as basic or neutral detergents such as the sulphonates and phenates, and preferred additives are basic magnesium or calcium sulphonates.
  • preferred additives are basic magnesium or calcium sulphonates.
  • the oils contain from 500 to 5000 parts per million of calcium and/or magnesium from such additives.
  • compositions of our invention may as an alternative or in addition contain other similar metal-containing detergent additives, for example, those containing barium, sodium, potassium or lithium.
  • the lubricating oil used in the lubricant composition may be a mineral lubricating oil or a synthetic lubricating oil or a mixture thereof.
  • Suitable synthetic oils include diester oils such as di(2-ethyl-hexyl) sebacate, azelate and adipate; complex ester oils such as those formed for dicarboxylic acids, glycols and either monobasic acids or monohydric alcohols; silicone oils; sulfide esters; organic carbonates; hydrocarbon oils and other synthetic oils known to the art.
  • the invention is particularly useful in mineral lubricating oils and has the added benefit that it may allow use of base stock oils that have inferior antioxidant properties to those currently used.
  • the lubricating compositions of the present invention may and usually will contain other traditional lubricant additives provided that they are substantially zinc-free and phosphorus-free - for example, rust inhibitors such as oleic acid and its derivatives such as N-oleylsarcosine, and oleic acid dimers and trimers, lecithin, sorbitan mono-oleate, dodecyl succinic anhydride or ethoxylated alkyl phenols; pour point depressants such as copolymers of vinyl acetate with fumaric acid esters of coconut oil alcohols; and viscosity index improvers such as olefin copolymers or polymethacrylates.
  • rust inhibitors such as oleic acid and its derivatives such as N-oleylsarcosine, and oleic acid dimers and trimers, lecithin, sorbitan mono-oleate, dodecyl succinic anhydride or ethoxylated
  • supplementary antioxidants in addition to the zinc dialkyldithiophosphate are sometimes required to improve the oxidative stability of the oil.
  • These supplementary antioxidants are included especially when the basestock has poor oxidative stability; and typically the supplementary antioxidant is added to the oil in amounts from 0.1-1.5 wt %.
  • the supplementary antioxidants that are used include phenols, hindered-phenols, bis-phenols, and sulphurised phenols, catechol, alkylated catechols and sulphurised alkyl catechols, diphenylamine and alkyl diphenylamines and phenyl-1-naphthylamine and its alkylated derivatives.
  • Additives for lubricating oils are generally supplied as concentrates in oil for incorporation into the bulk lubricant.
  • the present invention therefore provides concentrates comprising an oil solution containing:
  • the concentrate may also contain other additives such as the detergents and viscosity index improvers previously described.
  • a particularly preferred concentrate also contains a magnesium and/or calcium containing additive and the invention therefore provides a concentrate which further comprises from 0.1 to 8 wt % of calcium and/or magnesium.
  • Seq. IIID engine test according to ASTM STP 315M Part II in which the maximum and average cam plus lifter wear are measured. A pass in this test is achieved with maximum wear of 0.02 cm (0.008 in.) or better, and an average wear of 0.01 cm (0.004 in.) or better.
  • Kinematic viscosity increase in the IIID was measured at 40°C as a percentage increase in 64 hours. A pass is achieved in this test by achieving a viscosity increase in 64 hours of not more than 375%.
  • CRC-L-38 Screener engine test based on ASTM STP 509A PE IV in which the bearing weight loss (BWL) is measured. A pass in this test is achieved with BWL of not more than 40 mg.
  • the Examples of the invention show that the performance of the formulations is not merely summation of the performance of individual additive, but gives a surprising improvement in antiwear, antioxidant and bearing corrosion performance, while having phosphorus levels below those commercially employed in conventional oils.
  • Concentrates may also contain some dilute oil to improve handling (reduce viscosity).

Claims (33)

  1. Composition de lubrifiant pour carter destinée à être utilisée dans des moteurs de véhicules automobiles, comprenant une quantité dominante d'une huile lubrifiante, 5 à 500 parties par million en poids (ppm) de cuivre ajouté présent sous une forme soluble dans l'huile, un ou plusieurs composés ajoutés contenant du soufre, solubles dans l'huile, de manière que la composition renferme plus de 0,5 à 2,0 % en poids de soufre total, et un inhibiteur de corrosion des paliers, la composition contenant moins de 0,05 % en poids de phosphore et moins de 0,01 % en poids de zinc.
  2. Composition suivant la revendication 1, dans laquelle la quantité de cuivre ajouté dans la composition est de 10 à 400 ppm.
  3. Composition suivant la revendication 2, dans laquelle la quantité de cuivre ajouté dans la composition est de 10 à 200 ppm.
  4. Composition suivant la revendication 3, dans laquelle la quantité de cuivre ajouté dans la composition est de 60 à 200 ppm.
  5. Composition suivant l'une quelconque des revendications précédentes, dans laquelle du cuivre peut être incorporé dans l'huile sous forme du sel de cuivre d'un acide gras en C₁₀ à C₁₈, d'un acide carboxylique non saturé, d'un acide naphténique de poids moléculaire allant de 200 à 500 ou d'un acide dicarboxylique à substituant alkyle ou alcényle, d'un dithiocarbamate de cuivre soluble dans l'huile de formule générale (RR'NCSS)nCu dans lequel n a la valeur 1 ou 2 et R et R' sont des radicaux hydrocarbyle identiques ou différents contenant 1 à 18 atomes de carbone, un sulfonate de cuivre, un phénate de cuivre ou un acétylacétonate de cuivre.
  6. Composition suivant l'une quelconque des revendications précédentes, dans laquelle le composé de soufre soluble dans l'huile est un dithiocarbamate de formule (RR'NCSS)n M (dans laquelle R, R' et n sont tels que définis dans la revendication 5 et M est un métal) ou un mercaptide, un composé organique non saturé sulfuré, un sulfure, un thioéther, un thiophénol, un thioxanthate, un ester sulfuré, un thioester, un thioamide, un thiazole ou un thiadiazole.
  7. Composition suivant la revendication 6, dans laquelle le composé de soufre soluble dans l'huile est un dialkyl-dithiocarbamate contenant 2 à 12 atomes de carbone.
  8. Composition suivant l'une quelconque des revendications précédentes, qui contient plus de 0,5 à 1,0 % en poids de soufre total, comprenant 0,1 à 0,5 % en poids de soufre sous forme d'un composé ajouté contenant du soufre, soluble dans l'huile.
  9. Composition suivant l'une quelconque des revendications précédentes, qui est principalement dépourvue de zinc.
  10. Composition suivant la revendication 6, qui contient 0,5 à 3 % en poids d'ester sulfuré.
  11. Composition suivant l'une quelconque des revendications précédentes, dans laquelle l'inhibiteur de corrosion des paliers comprend un ou plusieurs esters boriques de formule :



            B(OR)₃ ou (RO)₂B-O-B(OR)₂, (ROBO)₃ ou (RO)₂BO-R¹-OB(OR)₂



    (où R est un groupe alkyle, aryle ou aralkyle substitué ou non substitué ou bien deux groupes R forment conjointement un groupe alkylène substitué ou non substitué et R¹ est un groupe alkylène substitué ou non substitué) et/ou un polysulfure de thiadiazole contenant 5 à 50 atomes de carbone ou un dérivé ou polymère de ce composé.
  12. Composition suivant la revendication 11, qui contient 0,01 à 10 % en poids d'un ester d'acide borique.
  13. Composition suivant la revendication 11 ou la revendication 12, dans laquelle l'ester d'acide borique est un orthoborate de tris(éthoxyéthyle) ou un biborate de butane-1,3,-diol.
  14. Composition suivant la revendication 11, qui contient 0,01 à 10 % en poids de 2,5-bis(tertio-nonyl-dithio)-1,3,4-thiadiazole.
  15. Composition suivant l'une quelconque des revendications précédentes, qui contient moins de 0,005 % en poids de phosphore.
  16. Composition suivant la revendication 15, qui est principalement dépourvue de phosphore.
  17. Composition suivant l'une quelconque des revendications précédentes, qui comprend en outre :
    (A) 1 à 10 % en poids d'un composé dispersant sans cendre et/ou
    (B) 0,3 à 10 % en poids d'un dispersant-agent améliorant l'indice de viscosité polymérique contenant de l'azote ou une fonction ester.
  18. Composition suivant l'une quelconque des revendications précédentes, qui comprend 2 à 8000 parties par million de calcium et/ou de magnésium.
  19. Composition suivant la revendication 18, qui comprend 500 à 5000 parties par million de calcium et/ou de magnésium sous forme de sulfonate basique de calcium et/ou de magnésium.
  20. Composition suivant l'une quelconque des revendications précédentes, qui comprend en outre un ou plusieurs additifs tels que des inhibiteurs de rouille, des agents abaissant le point d'écoulement, d'autres antioxydants et des agents améliorant l'indice de viscosité.
  21. Concentré comprenant une solution dans l'huile, contenant :
    (1) moins de 0,1 % en poids de phosphore ; et moins de 0,1 % en poids de zinc ;
    (2) 1 à 50 % en poids d'un composé contenant du soufre soluble dans l'huile ;
    (3) 0,005 à 2 % en poids de cuivre ;
    (4) 0,1 à 20 % en poids d'un inhibiteur de corrosion des paliers ; et
    (5) 0 à 60 % en poids d'un dispersant sans cendre et/ou 0 à 40 % en poids d'un agent polymérique dispersant-améliorant l'indice de viscosité.
  22. Concentré suivant la revendication 21, qui comprend en outre 0,01 à 8 % en poids de calcium et/ou de magnésium.
  23. Procédé de préparation d'une composition lubrifiante pour carter destinée à être utilisée dans des moteurs de véhicules automobiles, qui consiste à mélanger une quantité dominante d'une huile lubrifiante, du cuivre ajouté de manière que la composition comprenne 5 à 500 parties par million en poids (ppm) de cuivre ajouté présent sous une forme soluble dans l'huile, un ou plusieurs composés sulfurés ajoutés solubles dans l'huile de manière que la composition comprenne plus de 0,5 à 2,0 % en poids de soufre total, et un inhibiteur de corrosion des paliers, les substances à mélanger étant choisies de manière que la composition contienne moins de 0,05 % en poids de phosphore et moins de 0,01 % en poids de zinc.
  24. Procédé suivant la revendication 23, dans lequel la quantité de cuivre ajouté dans la composition va de 60 à 200 ppm.
  25. Procédé suivant la revendication 23 ou la revendication 24, dans lequel le composé de soufre soluble dans l'huile est un dialkyl-dithiocarbamate contenant 2 à 12 atomes de carbone.
  26. Procédé suivant l'une quelconque des revendications 23 à 25, dans lequel la proportion d'un ou plusieurs composés sulfurés ajoutés solubles dans l'huile est choisie de manière que la composition contienne plus de 0,5 à 1,0 % en poids de soufre total, y compris 0,1 à 0,5 % en poids de soufre sous forme de composé sulfuré ajouté soluble dans l'huile.
  27. Procédé suivant l'une quelconque des revendications 23 à 26, dans lequel les substances à mélanger sont choisies de manière que la composition soit principalement dépourvue de zinc.
  28. Procédé suivant l'une quelconque des revendications 23 à 27, dans lequel l'inhibiteur de corrosion des paliers comprend un ou plusieurs esters d'acide borique de formule :



            B(OR)₃, (RO)₂B-O-B(OR)₂, (ROBO)₃ ou (RO)₂BO-R¹-OB(OR)₂



    (où R est un groupe alkyle, aryle ou aralkyle substitué ou non substitué, ou bien deux groupes R forment conjointement un groupe alkylène substitué ou non substitué et R¹ est un groupe alkyène substitué ou non substitué) et/ou un polysulfure de thiadiazole contenant 5 à 50 atomes de carbone, un dérivé ou polymère de ce composé, l'ester d'acide borique ou le thiadiazole étant de préférence adjoint en une proportion de 0,01 à 10 % en poids sur la base de la composition finale.
  29. Procédé suivant l'une quelconque des revendications 23 à 28, dans lequel les substances à mélanger sont choisies de manière que la composition soit principalement dépourvue de phosphore.
  30. Procédé suivant l'une quelconque des revendications 23 à 29, dans lequel un ou plusieurs de (A), (B), (C) et (D) sont aussi incorporés dans la composition :
    (A) 1 à 10 % en poids d'un composé dispersant sans cendre ;
    (B) 0,3 à 10 % en poids d'un agent dispersant-améliorant l'indice de viscosité polymérique contenant de l'azote ou des groupes ester ;
    (C) 2 à 8000 parties par million de calcium et/ou de magnésium ; et
    (D) un ou plusieurs inhibiteurs de rouille, agents abaissant le point d'écoulement, anti-oxydants additionnels et agents améliorant l'indice de viscosité.
  31. Procédé de préparation d'un concentré, qui consiste à mélanger avec l'huile, pour former une solution, un ou plusieurs composés contenant du soufre solubles dans l'huile, un ou plusieurs composés contenant du cuivre, un inhibiteur de corrosion des paliers et, à titre facultatif, une ou plusieurs substances additionnelles choisies entre des composés contenant du phosphore, des dispersants sans cendre, des composés de calcium et des composés de magnésium, les proportions des substances mélangées étant telles que le concentré contient :
    (1) moins de 0,1 % en poids de phosphore ; et moins de 0,1 % en poids de zinc ;
    (2) 1 à 50 % en poids d'un composé contenant du soufre soluble dans l'huile ;
    (3) 0,005 à 2 % en poids de cuivre ;
    (4) 0,1 à 20 % en poids d'un inhibiteur de corrosion des paliers ;
    (5) 0 à 60 % en poids d'un dispersant sans cendre et/ou 0 à 40 % en poids d'un agent polymérique dispersant-améliorant l'indice de viscosité ; et à titre facultatif,
    (6) 0,01 à 8 % en poids de calcium et/ou de magnésium.
  32. Utilisation de cuivre soluble dans l'huile comme antioxydant dans une composition lubrifiante dépourvue de zinc et dépourvue de phosphore, comprenant un composé contenant du soufre soluble dans l'huile de manière que la composition renferme plus de 0,5 à 2,0 % en poids de soufre total, un inhibiteur de corrosion des paliers, un dispersant sans cendre et/ou un agent polymérique dispersant-améliorant l'indice de viscosité, et un détergent contenant du calcium et/ou du magnésium, le cuivre étant utilisé en quantité telle que la composition renferme 5 à 500 ppm de cuivre ajouté, présent sous une forme soluble dans l'huile.
  33. Utilisation d'une composition de lubrifiant pour carter, pour moteurs de véhicules automobiles, qui contient moins de 0,05 % en poids de phosphore et moins de 0,01 % en poids de zinc, 5 à 500 ppm de cuivre ajouté présent sous une forme soluble dans l'huile, plus de 0,5 à 2,0 % en poids de soufre total, et un inhibiteur de corrosion des paliers pour limiter l'oxydation, l'usure et la corrosion et pour satisfaire au moins aux normes de qualité de la catégorie SF et/ou CD des Engine Service Categories de l'API.
EP88301711A 1987-02-27 1988-02-26 Lubrifiants ayant une teneur basse en phosphore et zinc Expired - Lifetime EP0280579B1 (fr)

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GB8704683 1987-02-27
GB878704683A GB8704683D0 (en) 1987-02-27 1987-02-27 Low phosphorus/zinc lubricants

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EP0280579A3 EP0280579A3 (en) 1989-03-15
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US8030257B2 (en) 2005-05-13 2011-10-04 Exxonmobil Research And Engineering Company Catalytic antioxidants

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NO174211C (no) 1994-03-30
MX170236B (es) 1993-08-12
GR3007044T3 (fr) 1993-07-30
NO880847L (no) 1988-08-29
GB8704683D0 (en) 1987-04-01
KR880010107A (ko) 1988-10-07
JP2698367B2 (ja) 1998-01-19
ZA881260B (en) 1988-08-22
AU1234288A (en) 1988-09-01
KR960014934B1 (ko) 1996-10-21
ATE82316T1 (de) 1992-11-15
DK104088A (da) 1988-08-28
BR8800836A (pt) 1988-10-04
DK104088D0 (da) 1988-02-26
JPS63304095A (ja) 1988-12-12
DE3875755D1 (de) 1992-12-17
ES2036672T3 (es) 1993-06-01
MY103222A (en) 1993-05-29
DE3875755T2 (de) 1993-03-25
CA1306740C (fr) 1992-08-25
NO880847D0 (no) 1988-02-26
AU608295B2 (en) 1991-03-28
EP0280579A2 (fr) 1988-08-31
NO174211B (no) 1993-12-20
EP0280579A3 (en) 1989-03-15

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