EP0976813B1 - Additif contenant du borate pour huile de transmission manuelle stable à l'hydrolyse et assurant une durabilité élevée aux boítes de vitesse synchronisées - Google Patents

Additif contenant du borate pour huile de transmission manuelle stable à l'hydrolyse et assurant une durabilité élevée aux boítes de vitesse synchronisées Download PDF

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Publication number
EP0976813B1
EP0976813B1 EP98401967A EP98401967A EP0976813B1 EP 0976813 B1 EP0976813 B1 EP 0976813B1 EP 98401967 A EP98401967 A EP 98401967A EP 98401967 A EP98401967 A EP 98401967A EP 0976813 B1 EP0976813 B1 EP 0976813B1
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EP
European Patent Office
Prior art keywords
oil
extreme pressure
water
pressure additive
pentaerythritol
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
EP98401967A
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German (de)
English (en)
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EP0976813A1 (fr
Inventor
Pierre Tequi
Jacques Cazin
Daniel Vignerot
Christophe Le Sausse
Dominique Batelier
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Chevron Oronite SAS
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Chevron Oronite SAS
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Priority to EP98401967A priority Critical patent/EP0976813B1/fr
Priority to DE69820429T priority patent/DE69820429T2/de
Priority to CA002273613A priority patent/CA2273613C/fr
Priority to SG1999003707A priority patent/SG72973A1/en
Priority to JP21762999A priority patent/JP4460087B2/ja
Publication of EP0976813A1 publication Critical patent/EP0976813A1/fr
Application granted granted Critical
Publication of EP0976813B1 publication Critical patent/EP0976813B1/fr
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    • 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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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
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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
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • 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
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/041—Triaryl phosphates
    • 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
    • C10N2040/02—Bearings
    • 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
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • 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
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/042—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for automatic transmissions
    • 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
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/044—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for manual transmissions
    • 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
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/046—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for traction drives
    • 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
    • C10N2040/08—Hydraulic fluids, e.g. brake-fluids
    • 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
    • C10N2040/20—Metal working
    • 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
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • 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
    • C10N2040/20—Metal working
    • C10N2040/241—Manufacturing joint-less pipes
    • 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
    • C10N2040/20—Metal working
    • C10N2040/242—Hot working
    • 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
    • C10N2040/20—Metal working
    • C10N2040/243—Cold working
    • 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
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/245—Soft metals, e.g. aluminum
    • 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
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/246—Iron or steel
    • 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
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/247—Stainless steel
    • 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

  • the present invention relates to extreme pressure (EP) additives for lubricating oils.
  • EP extreme pressure
  • Especially the invention relates to a lubricant additive (preferably phosphorus free) for a manual transmission gear box containing potassium triborate having very good gear distress prevention properties, high synchromesh durability performance, and good water stability performance.
  • EP agents have been organic or metallo-organic compounds which are oil soluble or are easily incorporated as a stable dispersion in the oil.
  • Alkali metal borate is well known to the industry for its usefulness as a wear inhibitor and extreme pressure agent.
  • additives containing alkali metal borate may not be stable to hydrolysis.
  • alkali metal borate itself is slightly unstable in presence of water, the other components of the package such as friction modifiers, wear inhibitors, and metal deactivators deteriorate the hydrolysis stability of the lubricant. It is an object of the present invention to provide a lubricant having improved hydrolysis stability, while preventing gear distress, protecting the gear against fatigue, and having a high synchromesh durability. This last property is of paramount importance for manual transmission fluids.
  • the present invention provides an extreme pressure additive that improves the water stability, oxidation control, high synchromesh durability performance, and gear protection of a lubricating oil in a manual transmission gear box.
  • That additive contains an alkali-metal borate, an organic polysulfide, an alkyl succinic acid ester of a polyol, and an overbased sulfurized alkyl or alkenyl salicylate.
  • the alkali-metal borate is present at a level of from 30% to 70%.
  • the alkali-metal borate is potassium triborate present at a level of from 40% to 66%.
  • the organic polysulfide is present at a level of from 10% to 30%.
  • the organic polysulfide is a di-tertiary-butyl-polysulfide present at a level of from 12% to 25%.
  • the alkyl succinic acid ester of a polyol is present at a level of from 1% to 20%.
  • the alkyl succinic acid ester is the reaction product of pentaerythritol and polyisobutenyl succinic anhydride, and the alkyl succinic acid ester is present at a level of from 5% to 15%.
  • the overbased sulfurized alkyl or alkenyl salicylate is present at a level of from 0.5% to 20%.
  • the overbased sulfurized alkyl or alkenyl salicylate is an overbased mixture of a sulfurized alkyl salicylate and a sulfurized alkyl phenate, present at a level of from 5% to 10%.
  • the extreme pressure additive also has up to 20% of a fatty acid ester of a polyol, more preferably a pentaerythritol mono-oleate present at a level of from 5% to 10%.
  • the extreme pressure additive also contains up to 20% of an alkyl substituted phenyl phosphate, up to 7% of at least one metal deactivator, and up to 0.1% foam inhibitor.
  • the alkyl substituted phenyl phosphate is trixylenyl phosphate present at a level of from 5% to 10%.
  • At least one metal deactivator is used, more preferably more than one metal deactivator.
  • both 2,5-dimercapto-1,3,4-thiadiazole and benzotriazole derivative can be used.
  • the extreme pressure additive can be used in a lubricating oil composition with a base oil of lubricating viscosity.
  • That lubricating oil composition can also contain a viscosity index improver and a pour point depressant.
  • the high synchromesh durability performance and gear protection of a manual transmission gear box can be improved by adding to the gear box that lubricating oil.
  • the extreme pressure additive can also be used in a concentrate comprising a compatible organic liquid diluent and the extreme pressure additive.
  • the present invention involves an extreme pressure additive comprising an alkali-metal borate, an organic polysulfide, an alkyl succinic acid ester of a polyol, and an overbased sulfurized alkyl or alkenyl salicylate.
  • the additive can further comprise a fatty acid ester of a polyol.
  • the additive can further comprise an alkyl substituted phenyl phosphate, at least one metal deactivator, and a foam inhibitor.
  • the high synchromesh durability performance and gear protection of a manual transmission gear box can be provided by adding to the gear box a lubricating oil composition having improved water stability and oxidation control.
  • That lubricating oil composition comprises a base oil of lubricating viscosity and the extreme pressure additive as described above.
  • One method of producing the extreme pressure additive comprises blending together:
  • the additive produced by that method might have a slightly different composition than the initial mixture, because the components may interact.
  • the components can be blended in any order and can be blended as combinations of components.
  • the additive contains from 30% to 70% of an alkali-metal borate, preferably from 40% to 66% potassium triborate.
  • alkali-metal borates are well known in the art and are available commercially. Representative patents disclosing suitable borates and methods of manufacture include U.S. Patent Nos.: 3,313,727; 3,819,521; 3,853,772; 3,907,601; 3,997,454; and 4,089,790. Particularly preferred are the hydrated potassium triborate microparticles having a boron-to-potassium molar ratio of about 2.5 to 4.5. At least 90% of the borate particles generally have a particle size lower than 0.39 ⁇ m.
  • Alkali metal borates are used for the protection of gears against wear (scoring, pitting, ridging, rippling), to provide an optimum friction coefficient, and to protect the synchronizer ring against wear.
  • the additive contains from 10% to 30% of organic polysulfide, preferably from 12% to 25% di-tertiary-butyl-trisulfide.
  • the organic polysulfide is characterized as having sulfide linkages from at least 2 to about 10 sulfur atoms, preferably 2 to 6 sulfur atoms, more preferably 2 to 4 sulfur atoms.
  • the organic polysulfides are generally di, tri, or tetrasulfide compositions with trisulfide compositions preferred.
  • the organic polysulfides contain from 10% to 60% sulfur, preferably from 20% to 50% sulfur, and more preferably around 44% sulfur.
  • the organic polysulfide molecule may be defined by the formula: R 1 -S x -R 2 with x being from 2 to 10.
  • R 1 and R 2 may be olefinic compounds or alkyl groups having from 3 to 30 carbon atoms.
  • the organic polysulfide is di-tertiary-butyl-trisulfide which contains around 44% sulfur.
  • Organic polysulfides are introduced in the formulation to provide extreme pressure properties to protect gears against distress.
  • the alkyl succinic acid ester of a polyol is present at a level of from 1% to 20%.
  • the alkyl succinic acid ester is the reaction product of pentaerythritol and polyisobutenyl succinic anhydride, and the alkyl succinic acid ester is present at a level of from 5% to 15%.
  • alkenyl or alkyl substituted succinic anhydrides involving the reaction of a polyolefin and a maleic anhydride has been described in the art.
  • the alkenyl or alkyl group has a number average molecular weight (Mn) of from 500 to 2500 and a Mw/Mn ratio of from 1 to 500.
  • Mn number average molecular weight
  • the alkenyl or alkyl substituent of the succinic anhydride reactant is preferably polymerized isobutene having a Mn of 500 to 1500. Most preferably, it is a polymerized isobutene having a Mn of from 850 to 1200.
  • polyisobutenyl succinic anhydride The process for producing polyisobutenyl succinic anhydride has been described in the US Patent No. 3,381,022.
  • the alkyl substituted succinic anhydride is reacted with polyhydric alcohol such as glycerol, pentaerythritol, and sorbitol.
  • polyhydric alcohol such as glycerol, pentaerythritol, and sorbitol.
  • the aliphatic polyhydric alcohol is pentaerythritol.
  • This compound is used to improve the stability to hydrolysis and the compatibility/miscibility of the other parts of the additive.
  • the overbased sulfurized alkyl or alkenyl salicylate is present at a level of from 0.5% to 20%.
  • it is an overbased mixture of a sulfurized alkylsalicylate and a sulfurized alkylphenate, and the mixture is present at a level of from 5% to 10%.
  • the salicylate part of that mixture is a single aromatic ring alkylsalicylate, as is described in the European Patent Application EP 0 786 448 A2.
  • the alkylphenols used to prepare the overbased sulfurized alkyl or alkenyl salicylate contain up to 85% of linear alkylphenol in mixture with at least 15% of branched alkylphenol in which the branched alkyl radical contains at least nine carbon atoms.
  • these alkylphenols contain from 35% to 85% of linear alkylphenol in mixture with from 15% to 65% of branched alkylphenol.
  • the ratio of branched versus linear alkylphenol is given by weight.
  • the linear alkyl radical contains 12 to 40 carbon atoms, more preferably from 18 to 30 carbon atoms, and the branched alkyl radical contains at least 9 carbon atoms, preferably from 9 to 24 carbon atoms, more preferably 10 to 15 carbon atoms.
  • This compound is used to improve the stability to hydrolysis and to improve the thermal stability and the control of oxidation.
  • the fatty acid ester of a polyol is present at a level of up to 20%.
  • it is pentaerythritol mono-oleate present at a level of from 5% to 10%.
  • esters useful for this invention are oil-soluble and are preferably prepared from C 8 to C 22 fatty acids of the formula R-COOH wherein R is alkyl or alkenyl.
  • the preferred esters are obtained from oleic acids: C 16-18 and C 18 -unsaturated.
  • the ester is synthesized from the previously described fatty acids and polyols such as pentaerythritol, glycerol, sorbitol, etc.
  • This compound is used to have good friction properties, especially to provide good conditions for synchronization, and to improve the stability to hydrolysis.
  • the alkyl substituted phenyl phosphate is present at a level of up to 20%. Preferably it is trixylenyl phosphate present at a level of from 5% to 10%.
  • the phenol derivative used to obtain this phosphate may be cresol, xylenol, or tri-butyl-phenol.
  • This compound is used for its wear inhibition properties, especially for the protection of the synchronizer ring.
  • the metal deactivator is present at a level of up to 7%.
  • it is a mixture of a 2,5-dimercapto-1,3,4-thiadiazole derivative and a benzotriazole.
  • the 2,5-dimercapto-1,3,4-thiadiazole derivative is present at a level of up to 3.5% (preferably from 1% to 3%).
  • the benzotriazole is present at a level of up to 3.5% (preferably from 0.5 to 1.5%).
  • the 2,5 dimercapto-1,3,4,-thiadiazole derivative has the following formula
  • X may be an R ⁇ S or an R ⁇ S ⁇ S group with R being an alkyl group.
  • the 2,5 dimercapto-1,3,4,-thiadiazole derivative is used as a metal deactivator to prevent copper corrosion and as an extreme pressure agent.
  • the benzotriazole derivative is a mixture of the N,N-bis (2-ethylhexyl)-4-methyl-1H-benzotriazole-1-methylamine and N,N-bis (2-ethylhexyl)-5-methyl-1H-benzotriazole-1-methylamine. If desired, the benzotriazole derivative can be replaced with a tolutriazole derivative.
  • the benzotriazole derivative is used as a metal deactivator to prevent the corrosion of copper.
  • the foam inhibitor is present at a level of up to 0.1%.
  • the foam inhibitor contains about 3.5% silicon.
  • the additives produced by the process of this invention are useful for improving the water stability and oxidation control of lubricating oil compositions.
  • the amount of the additive ranges from about 0.5% to 40% of the total lubricating oil composition, although preferably from about 1% to 25% of the total lubricating oil composition.
  • the lubricating oil composition comprises a base oil of lubricating viscosity and the extreme pressure additive of the present invention.
  • the lubricating oil composition can also comprise viscosity index improvers and pour point depressants.
  • Examples of well-known viscosity index improvers include polymethacrylate type polymers, ethylene-propylene copolymers, styrene-isoprene copolymers, hydrated styrene-isoprene copolymers, polyisobutylene, and dispersant type viscosity index improvers.
  • pour point depressant is polymethyl methacrylate.
  • the oil of lubricating viscosity in which the extreme pressure additive is dispersed can be any fluid of low dielectric constant which is inert under the reaction conditions (particularly nonsaponiflable) and of lubricating viscosity.
  • Fluids of lubricating viscosity generally have viscosities of from 35 to 50,000 Saybolt Universal Seconds (SUS) at 100°F (38°C).
  • the fluid medium or oil may be derived from either natural or synthetic sources. Included among the natural hydrocarbonaceous oils are paraffin base, naphthenic base and mixed base oils. Synthetic oils include polymers of various olefins (generally from 2 to 6 carbon atoms), alkylated aromatic hydrocarbons, etc.
  • Nonhydrocarbon oils include polyalkylene oxides such as polyethylene oxide, aromatic ethers, silicone, etc.
  • the preferred media are the hydrocarbonaceous oils, both natural and synthetic.
  • Preferred among the hydrocarbonaceous oils are those having SAE viscosity numbers of 5W to 20W and 20W to 250W, and especially those having SAE viscosity numbers in the range 75W to 250W.
  • the content of the oil of lubricating viscosity in the lubricating oil composition will depend on the concentrations of the other components.
  • the lubricating oil constitutes the balance of the composition after the concentrations of the borate, the antiwear agents and the organic sulfur compounds and any other desired additives have been specified.
  • Additive concentrates are also included within the scope of this invention.
  • the concentrates of this invention comprise sufficient organic diluent to make them easy to handle during shipping and storage.
  • Suitable organic diluents which can be used include for example, solvent refined 100N, i.e., Cit-Con 100N, and hydrotreated 100N, i.e., RLOP 100N, and the like.
  • the organic diluent preferably has a viscosity of from about 1 to about 20 cSt at 100°C.
  • the organic diluent will constitute less than 10% of the concentrate.
  • hydrolysis stability tests are to assess the stability of a fully formulated lubricant to hydrolysis. Up to 3% water may be introduced by accident in the gear box during car wash. The additive has to be stable enough to avoid chemical reactions with water. Two tests have been developed to measure the hydrolysis stability.
  • 3% water is mixed up manually with a fully formulated lubricant in a graduated cylinder.
  • the cylinder containing the oil and water is stored at ambient temperature for ten days. After ten days, the mixture is visually inspected looking at the aspect of the oil, and at the part of the additive which has reacted with water. This part has to be 1 ml or lower, and the lubricant has to remain clear, without haze or gel formation.
  • the additive package contained the following compounds: 60.55% potassium tri-borate, 15.14% di-tertiary-butyl-trisulfide containing 44% sulfur, 6.06% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 8.48% overbased sulfurized alkyl salicylate, 6.06% pentaerythritol mono-oleate, 2.42 % 2,5 dimercapto-1,3,4,-thiadiazole derivative, 1.21 % benzotriazole derivative which is a mixture of N,N-bis (2-ethylhexyl)-4-methyl-1H-benzotriazote-1-methylamine and N,N-bis (2-ethylhexyl)-5-methyl-1H-benzotriazole-1-methylamine, and 0.08% silicon-containing foam inhibitor.
  • the lubricant contained: 8.7% of a concentrate containing 95% of the above additive package and 5% of a 100N mineral oil, 9.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 82.1% mixture of 65% of a 90N mineral base oil and 35% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.8 cSt, and the dynamic viscosity at ⁇ 40°C was 45000 cP.
  • the described package demonstrated a good oil and water separation with very limited reaction with water at ambient temperature (22°C and at 60°C), even when 3% of water is added into the package. There was slight deposit at the interface between water and oil which was essentially due to water and oil emulsion. This performance was evaluated with the previously described in-house procedures.
  • the deposit was less than 1 ml, the free water was 2 ml, and the aspect of the oil was very clear.
  • the FZG test rig (CEC L-07-A-95).
  • the described package has provided an effective protection of gears' teeth against surface fatigue (pitting).
  • the protection against pitting was assessed through the FZG C pitting test run at 90°C. This test is well known in the industry.
  • the described package provided an effective protection of synchronizer's ring against wear.
  • the synchromesh durability performance of the described packages was measured with the FZG SSP 180 procedure using Audi B80 brass synchronizer. This procedure was run at twice the normal duration.
  • FZG SSP 180 (Audi B80 brass synchronizer) Hürth test rig Pass (x2) >100000 Axial wear 0.57 - 0.57 mm Axial wear 0.36 ⁇ 0.81mm Friction coefficient: Beginning:0.108/0.11 End: 0.099/0.095 FZG SSP 180 (Audi B80 brass synchronizer) Hürth test rig (200000 cycles) Pass >200000 Axial wear: 0.42 ⁇ 0.88 mm Friction coefficient: Beginning: 0.11 100000: 0.095 End: 0.098 ZF synchro test (Mo/steel synchronizer) Pass >100000 Downshift: Friction coefficient: 0.079 - 0.085 Axial wear: 0.2 mm Ring wear: 0.1mm Upshift: Friction coefficient: 0.072 - 0.077 Axial wear: 0.25 mm Ring wear: 0.1mm
  • the additive package contained the following compounds: 43.92% potassium tri-borate, 28.54% di-tertiary-butyl-trisulfide containing 44% sulfur, 10.98% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 7.69% overbased sulfurized alkyl salicylate, 5.49% pentaerythritol mono-oleate, 3.29% 2,5 dimercapto-1,3,4,-thiadiazole derivative, 0.09% a silicon-containing foam inhibitor.
  • the lubricant contained: 9.7% of a concentrate containing 94% of the above additive package and 6% of a 100N mineral oil, 9.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 81.1% a mixture of 65% of a 90N mineral base oil and 35% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.8 cSt, and the dynamic viscosity at -40°C is 45000 cP.
  • the described package demonstrated a good oil and water separation with very limited reaction with water at ambient temperature (22°C and at 60°C), even when 3% of water is added into the package. There was slight deposit at the interface between water and oil which was essentially due to water and oil emulsion. This performance was evaluated with the previously described in-house procedures.
  • the deposit In the first test (3% of water, oil stored at ambient temperature) the deposit was 1 ml, the free water was 2 ml, and the aspect of the oil was clear. In the second test (0.5% of water, oil stored at 60°C) the bottom was covered by oil/water emulsion and the aspect of the oil was clear.
  • the described package provided an effective protection of synchronizer's ring against wear.
  • the synchromesh durability performance of the described packages was measured with the FZG SSP 180 procedure using Audi B80 brass synchronizer procedure.
  • FZG SSP 180 (Audi B80 brass synchronizer) Hürth test rig Pass >100000 Axial wear 0.70 - 0.77 mm Friction coefficient: Beginning:0.107 End: 0.08
  • the additive package contained the following compounds: 65.72% potassium tri-borate, 16.44% di-tertiary-butyl-trisulfide containing 44% sulfur, 6.57% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 9.20% overbased sulfurized alkyl salicylate, 1.31% 2,5 dimercapto-1,3,4,-thiadiazole derivative, 0.66% benzotriazole derivative which is a mixture of N,N-bis (2-ethylhexyl)-4-methyl-1H-benzotriazole-1-methylamine and N,N-bis (2-ethylhexyl)-5-methyl-1H-benzotriazole-1-methylamine, and 0.10% silicon-containing foam inhibitor.
  • the lubricant contained: 8.0% of a concentrate containing 95% of the above additive package and 5% of a 100N mineral oil, 9.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 82.8% a mixture of 65% of a 90N mineral base oil and 35% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.8 cSt, and the dynamic viscosity at ⁇ 40°C is 45000 cP.
  • the described package demonstrated a good oil and water separation with very limited reaction with water at ambient temperature (22°C and at 60°C), even when 3% of water is added into the package. There was slight deposit at the interface between water and oil which was essentially due to water and oil emulsion. This performance was evaluated with the previously described in-house procedures.
  • the deposit In the first test (3% of water, oil stored at ambient temperature) the deposit was 1 ml, the free water was 2 ml, and the aspect of the oil was very clear.
  • the additive package contained the following compounds: 56.45% potassium tri-borate, 22.58% di-tertiary-butyl-trisulfide containing 44% sulfur, 5.65% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 7.90% overbased sulfurized alkyl salicylate, 5.65% pentaerythritol mono-oleate 1.13% 2,5 dimercapto-1,3,4,-thiadiazole derivative, 0.57% benzotriazole derivative which is a mixture of N,N-bis (2-ethylhexyl)-4-methyl-1H-benzotriazole-1-methytamine and N,N-bis (2-ethylhexyl)-5-methyl-1H-benzotriazole-1-methylamine, and 0.07% silicon-containing foam inhibitor.
  • the lubricant contained: 9.3% of a concentrate containing 95% of the above additive package and 5% of a 100N mineral oil, 9.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 81.5% a mixture of 65% of a 90N mineral base oil and 35% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.8 cSt, and the dynamic viscosity at ⁇ 40°C is 45000 cP.
  • the described package demonstrated a good oil and water separation with very limited reaction with water at ambient temperature (22°C and at 60°C), even when 3% of water is added into the package. There was slight deposit at the interface between water and oil which was essentially due to water and oil emulsion. This performance was evaluated with the previously described in-house procedures.
  • the deposit was less than 1 ml, the free water was 2 ml, and the aspect of the oil was clear.
  • the described package has provided an effective protection of gears' teeth against surface fatigue (pitting).
  • the protection against pitting was assessed through the FZG C pitting test run at 90°C. This test is well known in the industry.
  • the described package provided an effective protection of synchronizer's ring against wear.
  • the synchromesh durability performance of the described packages was measured with the FZG SSP 180 procedure using Audi B80 brass synchronizer. This procedure was run at twice the normal duration.
  • FZG SS P 180 Pass (Audi B80 brass synchronizer) >100000 Axial wear 0.34 - 0.8 mm Hürth test rig Friction coefficient: Beginning:0.102 End: 0.111 ZF synchro test Pass (Mo/steel synchronizer) >100000 Downshift: Friction coefficient: 0.082 - 0.085 Axial wear: 0.15 mm Ring wear: 0.1mm Upshift: Friction coefficient: 0.085 - 0.076 Axial wear: 0.2 mm Ring wear: 0.15mm
  • the additive package contained the following compounds: 60.55% potassium tri-borate, 15.14% di-tertiary-butyl-trisulfide containing 44% sulfur, 6.06% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 8.48% overbased sulfurized alkyl salicylate, 6.06% trixylenyl phosphate 2.42% 2,5 dimercapto-1,3,4,-thiadiazole derivative, 1.21 % benzotriazole derivative which is a mixture of N,N-bis (2-ethylhexyl)-4-methyl-1 H-benzotriazole-1-methylamine and N,N-bis (2-ethylhexyl)-5-methyl-1H-benzotriazole-1-methylamine, and 0.08% silicon-containing foam inhibitor.
  • the lubricant contained: 8.7% of a concentrate containing 95% of the above additive package and 5% of a 100N mineral oil, 9.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 82.1% a mixture of 65% of a 90N mineral base oil and 35% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.8 cSt, and the dynamic viscosity at ⁇ 40°C is 45000 cP.
  • the described package demonstrated a good oil and water separation with very limited reaction with water at ambient temperature (22°C and at 60°C), even when 3% of water is added into the package. There was slight deposit at the interface between water and oil which was essentially due to water and oil emulsion. This performance was evaluated with the previously described in-house procedures.
  • the deposit was less than 1 ml, the free water was 2 ml, and the aspect of the oil was very clear.
  • the described package provided a very effective protection of gears' teeth against adhesive wear and abrasive. This protection against gear distress has been assessed through the following test well known in the industry: The results of the FZG test rig CEC L-07-A-95, double speed: pass 12.
  • the described package provided an effective protection of synchronizer's ring against wear.
  • the synchromesh durability performance of the described packages was measured with the FZG SSP 180 procedure using Audi B80 brass synchronizer. This procedure was run at twice the normal duration.
  • the additive package contained the following compounds: 59.94% potassium tri-borate, 13.32% di-tertiary-butyl-trisulfide containing 44% sulfur, 13.32% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 6.66% overbased sulfurized alkyl salicylate, 6.66% pentaerythritol mono-oleate, and 0.10% silicon-containing foam inhibitor.
  • the lubricant contained: 8.0% of a concentrate containing 94% of the above additive package and 6% of a 100N mineral oil, 5.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 86.8% a mixture of 65% of a 90N mineral base oil and 35% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.2 cSt, and the dynamic viscosity at ⁇ 40°C is 60000 cP.
  • the described package demonstrated a good oil and water separation with very limited reaction with water at ambient temperature (22°C and at 60°C), even when 3% of water is added into the package. There was slight deposit at the interface between water and oil which was essentially due to water and oil emulsion. This performance was evaluated with the previously described in-house procedures.
  • the deposit In the first test (3% of water, oil stored at ambient temperature) the deposit was 1 ml, the free water was 2 ml, and the aspect of the oil was very clear.
  • the described package provided an effective protection of synchronizer's ring against wear.
  • the synchromesh durability performance of the described packages was measured with the ZF synchromesh procedure.
  • ZF synchro test Mo/steel synchronizer
  • Axial wear 0.30 mm Ring wear: 0.15mm
  • the additive package contained the following compounds: 57.09% potassium tri-borate, 21.40% di-tertiary-butyl-trisulfide containing 44% sulfur, 4.28% primary alcohol zinc dithiophosphate, 7.14% high molecular weight substituted imidazoline, 9.99% low over-based alkyl calcium sulfonate, and 0.10% silicon-containing foam inhibitor.
  • the lubricant contained: 7.4% of a concentrate containing 95% of the above additive package and 5% of a 100N mineral oil, 5.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 87.4% a mixture of 55% of a 90N mineral base oil and 45% of a 600N mineral base oil.
  • the SAE grade is 75W-80W
  • the kinematic viscosity at 100°C is around 7.2 cSt
  • the dynamic viscosity at ⁇ 40°C is 60000 cP.
  • the described package has demonstrated a poor oil and water separation with important reaction with water at ambient temperature 22°C and at 60°C. There was a lot of deposit at the interface between water and oil which was essentially due to the reaction of some compounds of the additive with water. This performance was evaluated with the previously described in-house procedures.
  • the deposit In the first test (3% of water, oil stored at ambient temperature) the deposit was 4 ml, the free water was 0 ml, and the aspect of the oil was very hazy.
  • the additive package contained the following compounds: 50.59% potassium tri-borate, 18.97% di-tertiary-butyl-trisulfide containing 44% sulfur, 12.65% the reaction product of a 950 Mw polyisobutene, succinic anhydride and pentaerythritol, 2.53% primary alcohol zinc dithiophosphate 6.32% high molecular weight substituted imidazoline, 8.85% high over-based alkyl calcium sulfonate, and 0.09% silicon-containing foam inhibitor.
  • the lubricant contained: 8.3% of a concentrate containing 95% of the above additive package and 5% of a 100N mineral oil, 5.0% polymethacrylate type viscosity index improver, 0.2% polymethacrylate type pour point depressant, 86.5% a mixture of 55% of a 90N mineral base oil and 45% of a 600N mineral base oil.
  • the SAE grade was 75W-80W, the kinematic viscosity at 100°C was around 7.2 cSt and the dynamic viscosity at -40°C was 60000 cP.
  • the described package had demonstrated a poor oil and water separation with important reaction with water at ambient temperature 22°C and at 60°C. There is a lot of deposit at the inter-face between water and oil which is essentially due to the reaction of some compounds of the additive with water. This performance was evaluated with the previously described in-house procedures.
  • the deposit In the first test (3% of water, oil stored at ambient temperature) the deposit was 1.5 ml, the free water was 0 ml, and the aspect of the oil was very hazy.
  • the described package provided an effective protection of synchronizer's ring against wear.
  • the synchromesh durability performance of the described packages was measured with the FZG SSP 180 procedure using Audi B80 brass synchronizer. This procedure was run at twice the normal duration.
  • FZG SSP 180 (Audi B80 brass synchronizer) Pass (x2) >100000 Axial wear 0.1 - 0.1 mm Hürth test rig >100000 Axial wear 0.40 - 0.90 mm ZF synchro test (Mo/steel synchronizer) pass >100000 Downshift: Friction coefficient: 0.078 - 0.091 Axial wear: 0.15 mm Ring wear: 0.1mm Upshift: Friction coefficient: 0.071 - 0.085 Axial wear: 0.2 mm Ring wear: 0.15mm

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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)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)

Claims (9)

  1. Additif extrême-pression comprenant :
    (a) de 30 % à 70 % d'un borate de métal alcalin, de préférence de 40 % à 66 % de triborate de potassium ;
    (b) de 10 % à 30 % d'un polysulfure organique, de préférence de 12 % à 25 % d'un di-tert-butyl-trisulfure ;
    (c) de 1 % à 20 % d'un ester de l'acide succinique alkylé d'un polyol, de préférence de 5 % à 15 % du produit réactionnel du pentaérythritol et de l'anhydride poly-iso-butényle succinique; et
    (d) de 0,5 % à 20 % d'un salicylate d'alkyle ou d' alkényle sulfuré superbasique, de préférence de 5 % à 10 % d'un mélange superbasique d'un alkylsalicylate sulfuré et d'un alkylphénate sulfuré.
  2. Additif extrême-pression selon la revendication 1 comprenant en outre :
    (e) jusqu'à 20 % d'un ester d'acide gras d'un polyol, de préférence de 5 % à 10 % de mono-oléate de pentaérythritol.
  3. Un additif extrême-pression selon la revendication 1 ou 2 comprenant en outre :
    (f) jusqu'à 20 % d'un phosphate de phényle substitué par un groupe alkyle, de préférence de 5 % à 10 % de phosphate de trixylényle ;
    (g) jusqu'à 7 % d'au moins un désactivateur de métaux, de préférence de 1% à 3 % de dérivé de 2,5-dimercapto-1,3,4-thiadiazole et de 0,5 % à 1,5 % d'un benzotriazole ; et
    (h) jusqu'à 0,1 % d'un agent antimousse.
  4. Additif extrême-pression selon l'une quelconque des revendications 1 à 3 comprenant :
    (a) de 40 % à 66 % de triborate de potassium ;
    (b) de 12 % à 25 % d'un di-tert-butyl-trisulfure ;
    (c) de 5 % à 15 % du produit réactionnel du pentaérythritol et de l'anhydride poly-iso-butényle succinique;
    (d) de 5 % à 10 % d'un mélange superbasique d'un alkylsalicylate sulfuré et d'un alkylphénate sulfuré ;
    (e) de 5 % à 10 % de mono-oléate de pentaérythritol ;
    (f) de 5 % à 10 % de phosphate de trixylényle ;
    (g) de 1 % à 3 % de 2,5-dimercapto-1,3,4-thiadiazole ;
    (h) de 0,5 % à 1,5 % de dérivé de benzotriazole ; et
    (i) jusqu'à 0,1 % d'un agent antimousse.
  5. Composition d'huile lubrifiante comprenant une huile de base de viscosité lubrifiante et l'additif extrême-pression revendiqué dans l'une quelconque des revendications 1 à 4.
  6. Composition d'huile lubrifiante selon la revendication 5 comprenant en outre un améliorant d'indice de viscosité et un abaisseur du point d'écoulement.
  7. Concentré comprenant un diluant liquide organique compatible et l'additif extrême-pression revendiqué dans l'une quelconque des revendications 1 à 4.
  8. Procédé qui apporte une haute performance relative à la longévité du dispositif de synchronisation et qui fournit une protection de l'engrenage d'une boíte de vitesse à commande manuelle, ledit procédé comprenant l'adjonction à ladite boíte à engrenages d'une composition d'huile lubrifiante possédant une stabilité à l'eau et un contrôle de l'oxydation améliorés, ladite composition d'huile lubrifiante comprenant une huile de base de viscosité lubrifiante et l'additif extrême-pression revendiqué dans l'une quelconque des revendications 1 à 4.
  9. Procédé pour produire un additif extrême-pression comprenant de mélanger ensemble :
    (a) de 40 % à 66 % de triborate de potassium ;
    (b) de 12 % à 25 % d'un di-tert-butyl-trisulfure ;
    (c) de 5 % à 15 % du produit réactionnel du pentaérythritol et de l'anhydride poly-iso-butényle succinique; et
    (d) de 5 % à 10 % d'un mélange superbasique d'un alkylsalicylate sulfuré et d'un alkylphénate sulfuré ;
    (e) de 5 % à 10 % de mono-oléate de pentaérythritol ;
    (f) de 5 % à 10 % de phosphate de trixylényle ;
    (g) de 1 % à 3 % de 2,5-dimercapto-1,3,4-thiadiazole ;
    (h) de 0,5 % à 1,5 % de dérivé de benzotriazole ; et
    (i) jusqu'à 0,1 % d'un agent antimousse.
EP98401967A 1998-07-31 1998-07-31 Additif contenant du borate pour huile de transmission manuelle stable à l'hydrolyse et assurant une durabilité élevée aux boítes de vitesse synchronisées Expired - Lifetime EP0976813B1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP98401967A EP0976813B1 (fr) 1998-07-31 1998-07-31 Additif contenant du borate pour huile de transmission manuelle stable à l'hydrolyse et assurant une durabilité élevée aux boítes de vitesse synchronisées
DE69820429T DE69820429T2 (de) 1998-07-31 1998-07-31 Gegen Hydrolyse beständiges Borat enthaltendes Handschaltgetriebe-Schmieröladditiv zum Erhöhen der Dauerhaftigkeit von Synchrongetrieben
CA002273613A CA2273613C (fr) 1998-07-31 1999-06-02 Borate contenant un additif pour que le lubrifiant de transmission manuelle soit stable a l'hydrolyse et fournissant une grande durabilite pour les synchroniseurs
SG1999003707A SG72973A1 (en) 1998-07-31 1999-07-29 Borate containing additive for manual transmission lubricant being stable to hydrolysis and providing high synchromesh durability
JP21762999A JP4460087B2 (ja) 1998-07-31 1999-07-30 加水分解に対して安定で高いシンクロメッシュ耐久性を与える手動変速機潤滑剤用ホウ酸塩含有添加剤

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP98401967A EP0976813B1 (fr) 1998-07-31 1998-07-31 Additif contenant du borate pour huile de transmission manuelle stable à l'hydrolyse et assurant une durabilité élevée aux boítes de vitesse synchronisées

Publications (2)

Publication Number Publication Date
EP0976813A1 EP0976813A1 (fr) 2000-02-02
EP0976813B1 true EP0976813B1 (fr) 2003-12-10

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EP98401967A Expired - Lifetime EP0976813B1 (fr) 1998-07-31 1998-07-31 Additif contenant du borate pour huile de transmission manuelle stable à l'hydrolyse et assurant une durabilité élevée aux boítes de vitesse synchronisées

Country Status (5)

Country Link
EP (1) EP0976813B1 (fr)
JP (1) JP4460087B2 (fr)
CA (1) CA2273613C (fr)
DE (1) DE69820429T2 (fr)
SG (1) SG72973A1 (fr)

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Also Published As

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EP0976813A1 (fr) 2000-02-02
CA2273613A1 (fr) 2000-01-31
SG72973A1 (en) 2000-05-23
CA2273613C (fr) 2008-10-07
DE69820429D1 (de) 2004-01-22
JP2000063870A (ja) 2000-02-29
DE69820429T2 (de) 2004-10-14
JP4460087B2 (ja) 2010-05-12

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