EP0088453B1 - Schmiermittelzusammensetzung - Google Patents

Schmiermittelzusammensetzung Download PDF

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Publication number
EP0088453B1
EP0088453B1 EP83102377A EP83102377A EP0088453B1 EP 0088453 B1 EP0088453 B1 EP 0088453B1 EP 83102377 A EP83102377 A EP 83102377A EP 83102377 A EP83102377 A EP 83102377A EP 0088453 B1 EP0088453 B1 EP 0088453B1
Authority
EP
European Patent Office
Prior art keywords
viscosity
molecular weight
fluids
low
lubricants
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP83102377A
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English (en)
French (fr)
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EP0088453A1 (de
Inventor
Raymond Frederick Watts
Frederick Charles Loveless
Walter Nudenberg
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Uniroyal Chemical Co Inc
Original Assignee
Uniroyal Chemical Co Inc
Uniroyal Inc
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Application filed by Uniroyal Chemical Co Inc, Uniroyal Inc filed Critical Uniroyal Chemical Co Inc
Publication of EP0088453A1 publication Critical patent/EP0088453A1/de
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    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/04—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/06—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds
    • C10M2223/065—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • 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
    • C10N2040/25—Internal-combustion engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C10N2040/251—Alcohol fueled engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C10N2040/255—Gasoline engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C10N2040/255—Gasoline engines
    • C10N2040/28—Rotary engines

Definitions

  • This invention relates to compositions useful as lubricating oils having high viscosity index, improved resistance to oxidative degradation and resistance to viscosity losses caused by permanent or temporary shear.
  • Object of the invention is to provide lubricating compositions exhibiting permanent shear stability, superior oxidative stability and excellent temperature-viscosity properties.
  • the invention comprises a lubricating composition comprising:
  • the invention comprises a lubricating composition comprising:
  • This second alternative composition can further comprise an ester having a viscosity of 1-10 mm 2 /s at 100°C.
  • the invention comprises a lubricating composition comprising:
  • This third alternative composition can further comprise an ester having a viscosity of 1-10 mm 2 /s at 100°C.
  • the invention comprises a lubrication composition comprising:
  • the second, third and fourth alternative composition can further comprise an additive package comprising at least one additive selected from the group consisting essentially of dispersants, oxidation inhibitors, corrosion inhibitors, anti-wear agents, pour point depressants, anti-rust agents, foam inhibitors and extreme pressure agents.
  • the viscosity-temperature relationship of a lubricating oil is one of the critical criteria which must be considered when selecting a lubricant for a particular application.
  • the mineral oils commonly used as a base for single and multigraded lubricants exhibit a relatively large change in viscosity with a change in temperature. Fluids exhibiting such a relatively large change in viscosity with temperature are said to have a low viscosity index.
  • the viscosity index of a common paraffinic mineral oil is usually given a value of about 100. Viscosity index (VIU) is determined according to ASTM Method D 2770-74 wherein the VI is related to kinematic viscosities measured at 40°C and 100°C.
  • Lubricating oils composed mainly of mineral oil are said to be single graded.
  • SAE grading requires that oils have a certain minimum viscosity at high temperatures and, to be multigraded, a certain maximum viscosity at low temperatures. For instance, an oil having a viscosity of 10 mm 2 /s at 100°C (hereinafter all viscosities are at 100°C unless otherwise noted) would be an SAE 30 and if that oil had a viscosity of 3400 m p a-s at -20°C, the oil would be graded 10W-30.
  • An unmodified mineral oil of 10 mm 2 /s can not meet the low temperature requirements for a 10W-30 multigrade rating, since its viscosity index dictates that it would have a viscosity considerably greater than 3500 mPa.s at -20°C, which is the maximum allowed viscosity for a 10W rating.
  • the viscosity requirements for qualification as multigrade engine oils are described by the SAE Engine Oil Viscosity Classification - SAE J300 SEP80, which became effective April 1, 1982.
  • the low temperature (W) viscosity requirements are determined by ASTM D 2602, Method of Test for Apparent Viscosity of Motor Oils at Low Temperature Using the Cold Cranking Simulator, and the results are reported in mPa. s.
  • the higher temperature (100°C) viscosity is measured according to ASTM D445, Method of Test for Kinematic Viscosity of Transparent and Opaque Liquids, and the results are reported in mm 2 /s.
  • the following table outlines the high and low temperature requirements for the recognized SAE grades for engine oils.
  • the 40°C viscosity estimated by linearly connecting the 100°C and -25°C viscosities would be about 70 mm 2 /s.
  • Polymeric thickeners are added to bring the viscosity of a base fluid up to that required for a certain SAE grade and to increase the viscosity index of the fluid, allowing the production of multigraded oils.
  • Polymeric VI improvers are traditionally high molecularweight rubbers whose molecular weights may vary from 10,000 to 1,000,000. Since the thickening power and VI increase are related to the molecular weight of the VI improver, most of these polymers normally have a molecular weight of at least 100,000.
  • Temporary shear is the result of the non-Newtonian viscometrics associated with solutions of high molecular weight polymers. It is caused by an alignment of the polymer chains with the shear field under high shear rates with a resultant decrease in viscosity. The decreased viscosity reduces the wear protection associated with viscous oils. Newtonian fluids maintain their viscosity regardless of shear rate.
  • Certain specific blends of high viscosity synthetic hydrocarbons, low viscosity synthetic hydrocarbons and optionally low viscosity esters form base fluids from which superior crankcase or gear oils can be produced by the addition of the proper additive "packages".
  • the finished oils thus prepared exhibit very high stability to permanent shear and, because of their Newtonian nature, very little, if any, temporary shear and so maintain the viscosity required for proper wear protection.
  • the oils of this invention have remarkably better stability toward oxidative degradation than those of the prior art.
  • the unexpectedly high viscosity indices produced from our base fluid blends permit the preparation of broadly multigraded crankcase ffluids, such as 5W-40 and gear oils such as 75W-140.
  • the high viscosity synthetic hydrocarbons having viscosities of 40 to 1000 mm 2 /s may be polyalphaolefins, ethylene-alphaolefin oligomers or hydrogenated polyisoprene oligomers.
  • the high viscosity polyalphaolefins of the present invention have viscosities of from 40 to 1000 mm 2 /s, preferably from 40 to 250 mm 2 /s, and are conveniently prepared by any of a series of methods described in the literature.
  • the catalysts employed are those commonly referred to as Friedel-Crafts catalysts. Such catalysts cause cationic oligomerization of alphaolefins, such as octene-1 or decene-1 to molecular weights ranging up to several thousand, depending on the catalyst and polymerization conditions employed.
  • Ziegler catalysts such as described in US-A-3,179,711 can also be used to prepare oligomers in the molecular weight range useful in this invention.
  • Polyalphaolefins can likewise be prepared with peroxide catalysts, BF 3 based catalysts and by thermal polymerization. These methods, however, generally produce only low molecular weight oligomers.
  • the high molecular weight polyalphaolefins of this invention are preferably hydrogenated to decrease their level of unsaturation and thereby to increase their stability toward oxidation.
  • the alphaolefins utilized to make the high viscosity oligomers of the invention can range from C 3 (propylene) to C 14 (tetradecene) or any mixtures, although oligomers of octene-1, decene-1 and dodecene-1 are preferred because of their high viscosity indices and low pour points.
  • the high viscosity ethylene-alphaolefin oligomers of this invention are conveniently prepared by Ziegler catalysis. Many references exist covering methods of producing liquid oligomers of ethylene and alphaolefins (particularly propylene).
  • Polymerization is typically performed by subjecting the monomer mixture usually in a solvent to the combination of an organo aluminum compound and a vanadium or titanium compound.
  • the products formed can range from materials having viscosities as low as 20 mm 2 /s to rubbery semi-solids depending on the choice of catalyst, the addition of molecular weight regulating species, temperature of polymerization and, especially, imposed hydrogen pressure.
  • low viscosity oligomers are prepared by the pyrolysis of high viscosity oligomers or rubbery solids.
  • Typical preparations of liquid ethylene-alphaolefin copolymers can be found in references, such as US-A-3,634,249, US-A-3,923,919, US-A-3,851,011, US-A-3,737,477, US-A-3,499,741, US-A-3,681,302, US-A-3,819,592, US-A-3,896,094, US-A-3,676,521, BE-A-570,843, US-A-3,068,306, and US-A-3,328,366.
  • oligomers of ethylene and at least one other alphaolefin of this invention may be hydrogenated to increase their stability toward oxidation, the proper choice of polymerization catalysts in the presence of hydrogen often produces oligomers having very low levels of unsaturation directly.
  • the alphaolefins which can be used singly or in combinations with ethylene include linear alphaolefins of C 3 (propylene) to C 14 (tetradecene) and branches alphaolefins of the same molecular weight range, provided that the branch point is at least in the beta position to the double bond (e.g. 4-methyl pentene-1).
  • propylene and the lower molecular weight olefins are the preferred monomers in the preparation of the oligomers of ethylene and at least one other alphaolefin of this invention.
  • the viscosity of the ethylene-alphaolefin oligomers of this invention is preferably 40 to 1000 mm 2 /s while the ethylene content is preferably 30 to 70 wt.%.
  • oligomeric ethylene-alphaolefin polymers which contain controlled amounts of unsaturation introduced by copolymerization with certain non-conjugated diene such as dicyclopentadiene, ethylidene norbornene and 1,4-hexadiene.
  • certain non-conjugated diene such as dicyclopentadiene, ethylidene norbornene and 1,4-hexadiene.
  • the introduction of unsaturation is sometimes desired if the oligomer is to be treated in any way to produce polar functionality thus giving the oligomer dispersant properties.
  • the oligomeric polyisoprenes of this invention may be prepared by Ziegler or, preferably, anionic polymerization. Such polymerization techniques are described in US-A-4,060,492.
  • the preferred method of preparation for the liquid hydrogenated polyisoprenes is by the anionic alkyl lithium catalyzed polymerization of isoprene.
  • alkyl lithium catalysts such as secondary butyl lithium results in a polyisoprene oligomer having a very high (usually greater than 80%) 1,4-content, which results in backbone unsaturation.
  • alkyl lithium catalysts When alkyl lithium catalysts are modified by the addition of ethers or amines, a controlled amount of 1,2- and 3,4- addition can take place in the polymerization. Hydrogenation of these structures gives rise to the saturated species represented below:
  • Structure A is the preferred structure because of its low Tg and because it has a lower percent of its mass in the pendant groups (CH 3 ⁇ ).
  • Structure B is deficient in that the tetrasubstituted carbons produced serve as points of thermal instability.
  • Structure C has 60% of its mass in a pendant (isopropyl) group which, if repeated decreases the thickening power of the oligomer for a given molecular weight and also raises the Tg of the resultant polymer. This latter property has been shown to correlate with viscosity index. Optimization of structure A is desired for the best combination of thickening power, stability and VI improvement properties.
  • alkyl lithium polymers Another feature of alkyl lithium polymers is the ease with which molecular weight and molecular weight distribution can be controlled.
  • the molecular weight is a direct function of the monomer to catalyst ratio and, taking the proper precautions to exclude impurities, can be controlled very accurately thus assuring good quality control in the production of such polymer.
  • The-alkyl lithium catalysts produce very narrow molecular weight distributions such that Mw/Mn ratios of 1.1 are easily gained.
  • VI improvers a narrow molecular weight distribution is highly desirable since, at the given molecular weight, thickening power is maximized while oxidative and shear instability are minimized.
  • broad or even polymodal M.W. distributions are easily produced by a variety of techniques well known in the art.
  • Star- shaped or branched polymers can also be readily prepared by the inclusion of multifunctional monomers such as divinyl benzene or by termination of the "living" chains with a polyfunctional coupling agent such as dimethylterephthalate
  • isoprene oligomers require hydrogenation to reduce the high level of unsaturation present after polymerization.
  • 90%, and preferably 99% or more of the olefinic linkages should be saturated.
  • the high viscosity synthetic hydrocarbons of this invention should have viscosities ranging from about 40 to about 1000 mm 2 /s.
  • the low viscosity synthetic hydrocarbons of the present invention having viscosities of from 1 to 10 cSt., consist primarily of oligomers of alphaolefins and alkylated benzenes.
  • Low molecular weight oligomers of alphaolefins from C a (octene) to C, 2 (dodecene) or mixtures of the olefins can be utilized.
  • Low viscosity alphaolefin oligomers can be produced by Ziegler catalysis, thermal polymerization, free radically catalyzed polymerization and, preferably, BF 3 catalyzed polymerization.
  • BF 3 catalyzed polymerization preferably, BF 3 catalyzed polymerization.
  • a host of similar processes involving BF 3 in conjunction with a cocatalyst is known in the patent literature.
  • a typical polymerization technique is described in US-A-4,045,508.
  • the alkyl benzenes may be used in the present invention alone or in conjunction with low viscosity polyalphaolefins in blends with high viscosity synthetic hydrocarbons and low viscosity esters.
  • the alkyl benzenes prepared by Friedel-Crafts alkylation of benzene with olefins are usually predominantly dialkyl benzenes wherein the alkyl chain may be 6 to 14 carbon atoms long.
  • the alkylating olefins used in the preparation of alkyl benzenes can be straight or branched chain olefins or combinations. These materials may be prepared as shown in US-A-3,909,432.
  • the low viscosity esters of this invention having viscosities of from 1 to 10 mm 2 /s can be selected from classes of esters readily available commercially, e.g., monoesters prepared from monobasic acids such as pelargonic acid and alcohols; diesters prepared from dibasic acids and alcohols or from diols and monobasic acids or mixtures of acids; and polyol esters prepared from diols, triols (especially trimethylol propane), tetraols (such as pentaerythritol), hexaols (such as dipentaerythritol) and the like reacted with monobasic acids or mixtures of acids.
  • monoesters prepared from monobasic acids such as pelargonic acid and alcohols
  • diesters prepared from dibasic acids and alcohols or from diols and monobasic acids or mixtures of acids
  • esters examples include tridecyl pelargonate, di-2-ethylhexyl adipate, di-2-ethylhexyl azelate, trimethylol propane triheptanoate and pentaerythritol tetraheptanoate.
  • esters and mixtures of esters derived from natural sources, plant or animal are those esters and mixtures of esters derived from natural sources, plant or animal. Examples of these materials are the fluids produced from jojoba nuts, tallows, safflowers and sperm whales.
  • esters used in our blends must be carefully selected to insure compatibility of all components in finished lubricants of this invention. If esters having a high degree of polarity (roughly indicated by oxygen content) are blended with certain combinations of high viscosity synthetic hydrocarbons and low viscosity synthetic hydrocarbons, phase separation can occur at low temperatures with a resultant increase in apparent viscosity. Such phase separation is, of course, incompatible with long term storage of lubricants under a variety of temperature conditions.
  • the additive "packages" mixed with the recommended base oil blend for the production of multigraded crankcase fluids or gear oils are usually combination of various types of chemical additives so chosen to operate best under the use conditions which the particular formulated fluid may encounter.
  • Additives can be classified as materials which either impart or enhance a desirable property of the base lubricant blend into which they are incorporated. While the general nature of the additives might be the same for various types or blends of the base lubricants, the specific additives chosen will depend on the particular type of service in which the lubricant is employed and the characteristics of the base lubricants.
  • a finished lubricant will contain several and possibly most or all of the above types of additives in what is commonly called an "additive package".
  • the development of a balanced additive package involves considerably more work than the casual use of each of the additive types. Quite often functional difficulties arising from combinations of these materials show up under actual operating conditions. On the other hand, certain unpredictable synergistic effects of a desirable nature may also become evident. The only methods currently available for obtaining such data are from extensive full scale testing both in the laboratory and in the field. Such testing is costly and time-consuming.
  • Dispersants have been described in the literature as “detergents”. Since their function appears to be one of effecting a dispersion of particulate matter, rather than one of "cleaning up” any existing dirt and debris, it is more appropriate to categorize them as dispersants.
  • Materials of this type are generally molecules having a large hydrocarbon "tail” and a polar group head.
  • the tail section an oleophilic group, serves as a solubilizer in the base fluid while the polar group serves as the element which is attracted to particulate contaminants in the lubricant.
  • the dispersants include metallic and ashless types.
  • the metallic dispersants include sulfonates (products of the neutralization of a sulfonic acid with a metallic base), thiophosphonates (acidic components derived from the reaction between polybutene and phosphous pentasulfide) and phenates and phenol sulfide salts (the broad class of metal phenates includes the salts of alkylphenols, alkylphenol sulfides, and alkyl phenol aldehyde products).
  • the ashless type dispersants may be categorized into two broad types: high molecular weight polymeric dispersants for the formulation of multigrade oils and lower molecular weight additives for use where viscosity improvement is not necessary.
  • the compounds useful for this purpose are again characterized by a "polar" group attached to a relatively high molecular weight hydrocarbon chain.
  • the "polar” group generally contains one or more of the elements- nitrogen, oxygen, and phosphorus.
  • the solubilizing chains are generally higher in molecular weight than those employed in the metallic types; however, in some instances they may be quite similar.
  • Some examples are N-substituted long chain alkenyl succinimides, high molecular weight esters, such as products formed by the esterification of mono or polyhydric aliphatic alcohols with olefin substituted succinic acid, and Mannich bases from high molecular weight alkylated phenols.
  • the high molecular weight polymeric ashless dispersants have the general formula:
  • an oxidation inhibitor is the prevention of a deterioration associated with oxygen attack on the lubricant base fluid. These inhibitors function either to destroy free radicals (chain breaking) or to interact with peroxides which are involved in the oxidation mechanism.
  • antioxidants are the phenolic types (chain-breaking) e.g., 2,6-di-tert.-butyl para cresol and 4,4'-methylenebis(2,6-di-tert.-butylphenol), and the zinc dithiophosphates (peroxide-destroying).
  • Wear is loss of metal with subsequent change in clearance between surfaces moving relative to each other. If continued, it will result in engine or gear malfunction.
  • the principal factors causing wear are metal-to-metal contact, presence of abrasive particulate matter, and attack of corrosive acids.
  • Metal-to-metal contact can be prevented by the addition of film-forming compounds which protect the surface either by physical absorption or by chemical reaction.
  • the zinc dithiophosphates are widely used for this purpose. These compounds were described under anti-oxidant and anti-bearing corrosion additives. Other effective additives contain phosphorus, sulfur or-combinations of these elements.
  • Abrasive wear can be prevented by effective removal of particulate matter by filtration while corrosive wear from acidic materials can be controlled by the use of alkaline additives such as basic phenates and sulfonates.
  • conventional viscosity improvers are often used in "additive packages" their use should not be necessary for the practice of this invention since our particular blends of high and low molecular weight base lubricants produce the same effect.
  • These materials are usually oil-soluble organic polymers with molecular weights ranging from approximately 10,000 to 1,000,000. The polymer molecule in solution is swollen by the lubricant. The volume of this swollen entity determines the degree to which the polymer increases its viscosity.
  • pour point depressants prevent the congelation of the oil at low temperatures. This phenomenon is associated with the crystallization of waxes from the lubricants. Chemical structures of representative commercial pour point depressants are:
  • Chemicals employed as rust inhibitors include sulfonates, alkenyl succinic acids, substituted imidazolines, amines, and amine phosphates.
  • the anti-foam agents include the silicones and miscellaneous organic copolymers.
  • Additive packages known to perform adequately for their recommended purpose are prepared and supplied by several major manufacturers. The percentage and type of additive to be used in each application is recommended by the suppliers. Typically available packages are:
  • a typical additive package for an automotive gear lubricant would normally contain antioxidant, corrosion inhibitor, anti-wear agents, anti-rust agents, extreme pressure agent and foam inhibitor.
  • a typical additive package for a crankcase lubricant would normally be comprised of a dispersant, antioxidant, corrosion inhibitor, anti-wear agent, anti-rust agent and foam inhibitor.
  • An additive package useful for formulating a compressor fluid would typically contain an anti-oxidant, anti-wear agent, an anti-rust agent and foam inhibitor.
  • This invention describes blends of high viscosity synthetic hydrocarbons, having a viscosity range of 40 to 1000 mm 2 /s with one or more synthetic hydrocarbon fluids having viscosities in the range of 1 to 10 mm 2 /s and/or one or more compatible ester fluids having a viscosity range of 1 to 10 mm 2 /s.
  • Such blends when treated with a properly chosen additive "package" can be formulated in multigraded crankcase or gear oils having superior shear stability, superior oxidative stability, and Newtonian viscometric properties.
  • the blends of this invention also find uses in certain applications where no additive need be employed.
  • the high viscosity synthetic hydrocarbon provides thickening and VI improvement to the base oil blend.
  • blends of high viscosity synthetic hydrocarbons with low viscosity synthetic hydrocarbons produce fluids having much greater oxidative stability than low viscosity synthetic hydrocarbons alone. This is illustrated in Example 7.
  • the VI improvement produced by high viscosity synthetic hydrocarbon in blends with low viscosity synthetic hydrocarbons or low viscosity esters is shown in Examples 8 and 9. These improvements persist in blends of high viscosity synthetic hydrocarbons, low viscosity synthetic hydrocarbons, and low viscosity esters.
  • the low viscosity synthetic hydrocarbon fluid is frequently the main ingredient in the base oil blend, particularly in finished lubricants having an SAE viscosity grade of 30 or 40. While certain low viscosity esters are insoluble in high viscosity synthetic hydrocarbons, the presence of low viscosity synthetic hydrocarbon, being a better solvent for low viscosity esters, permits greater variations in the type of esters used in base oil blends of high viscosity synthetic hydrocarbons, low viscosity synthetic hydrocarbons, and low viscosity esters.
  • Crankcase and gear oils consisting solely of hydrogenated polyisoprene oligomers and low viscosity synthetic hydrocarbons with the proper additives produce synthetic fluids having excellent oxidative and hydrolytic stability.
  • Such fluids are exemplified in Examples 22 and 23.
  • the third optional component, low viscosity esters can be used in combination with hydrogenated polyisoprene oligomers and low viscosity hydrocarbons or alone with hydrogenated polyisoprene oligomers.
  • the proper choice of ester and hydrogenated polyisoprene oliogmers can produce crankcase and gear oil formulations having outstanding viscosity indices and low temperature properties. Such three component blends are illustrated in Examples 24 and 25.
  • Two component blends of hydrogenated polyisoprene oligomers and esters can be used to prepare multigraded lubricants having outstanding viscometric properties, detergency, and oxidative stability. While some applications present environments having high moisture levels, which would be deleterious to certain esters, there are other applications such as automotive gear oils where the high ester contents found in the hydrogenated polyisoprene oligomers-ester blends can be used to advantage. Examples 26 and 27 illustrate the formulation of multigrade lubricants with such two component blends.
  • the low viscosity hydrocarbons act as a common solvent for the ethylene-alpha-olefin oligomers and the added ester. Depending on the polarity of the ester, the latter two are frequently somewhat incompatible. Excellent multigraded lubricants can be formulated with or without ester.
  • the third component, low viscosity esters can be added to produce the superior lubricants of this invention.
  • High viscosity synthetic hydrocarbons and low viscosity synthetic hydrocarbons can be used alone to produce multigraded lubricants.
  • the addition of low levels of low viscosity esters, usually 1-25% results in a base oil blend superior to blends of high viscosity synthetic hydrocarbons and low viscosity synthetic hydrocarbons alone in low temperature fluidity.
  • low viscosity esters usually constitute 10-25% of the synthetic base oil blend, more or less can be used in specific formulations. When the final application involves exposure to moisture elimination or limitation of the amount of ester in blends may be advantageous.
  • the components of the finished lubricants of this invention can be admixed in any convenient manner or sequence.
  • An important aspect of the present invention is in the use of the properly constituted base oil blend in combination with the proper compatible additive package to produce finished multigrade lubricants having:
  • the lubricants of this invention when properly formulated, display viscometrics of Newtonian fluids. That is, their viscosities are unchanged over a wide range of shear rates. While some of the high viscosity synthetic hydrocarbons of the invention may, in themselves, display non-Newtonian characteristics, particularly at low temperatures, the final lubricant products utilizing low viscosity oils as diluents are Newtonian. We have observed that synthetic hydrocarbons of up to 300 mm 2 /s are Newtonian at room temperature as shown by the absence of a Weissenberg effect. And while fluids of 500 to 1000 mm 2 /s do show a Weissenberg effect, solutions of such oligomers in quantities commonly used to attain Standard SAE viscosity grades do not.
  • the thickening fluids of high viscosity synthetic hydrocarbons of this invention all have molecular weights below 5000, and so, it should be obvious that shear thinning of their solutions would be nil. That is, they will display Newtonian character.
  • the shear rates developed in pistons and gears (equal to or greater than 10 6 sec- 1 ) is such that, depending on the polymeric thickener used, the apparent viscosity of the oils approaches that of the unthickened base fluids resulting in loss of hydrodynamic films. Since wear protection of moving parts has been correlated with oil viscosity, it is apparent that the wear characteristics of a lubricant can be downgraded as a result of temporary shear.
  • the Newtonian fluids of the current invention maintain their viscosity under these use conditions and therefore afford more protection to and hence longer lifetime for the machinery being lubricated.
  • Example 10 illustrates the oxidation of a low viscosity fluid thickened with 100 mm 2 /s polyalphaolefin and compares it with the same fluid thickened with a commercial VI improver.
  • Example 11 further compares the oxidative stability of fully formulated lubricants of this invention with two nearly identical lubricant formulations, except that the latter are thickened with commercial VI improver.
  • lubricating oils of this invention are superior to traditional multigraded lubricants because of their greater resistance to permanent shear and oxidation.
  • the prolonged "stay in grade” performance of our lubricating fluids offers advances in durability of machinery using such fluids.
  • the advantages a Newtonian fluid brings to such a grading system are obvious to anyone skilled in the art.
  • the viscosity of a Newtonian fluid can be directly extrapolated to 150°C under high shear conditions.
  • a polymer thickened fluid will invariably have a viscosity lower than the extrapolated value, frequently close to the base fluid itself.
  • polymer thickened oils will require a more viscous base fluid.
  • the use of thicker base fluids will produce higher viscosities at low temperature making it more difficult to meet the low temperature (5W for crankcase of 75W for gear oil) requirements for broadly multigraded oils.
  • Viscosity index is determined by low shear viscosity measurements at 40°C and 100°C.
  • the Newtonian lubricants of this invention not only produce high viscosity index multigraded fluids which stay "in grade", but the VI and multigrade rating are realistic since they are not sensitive to shear.
  • This example illustrates the preparation of multigraded gear oils utilizing high viscosity polyalphaolefin (PAO) as a thickener.
  • PAO high viscosity polyalphaolefin
  • the oil For a 80W-140 oil the oil must have a minimum viscosity at 100°C of 24 cSt. and a viscosity of 150,000 cP. or less at -26°C.
  • This example illustrates preparation of gasoline and diesel crankcase lubricants.
  • This example illustrates the excellent oxidative stability of gear oils utilizing high molecular weight PAO.
  • a 75W-90 gear oil prepared as in Example 1.B.D. was subjected to the CRC L-60 Thermal Oxidation Stability Test. In this test 120 ml of oil are heated to 325° ⁇ 1°F and 11.1 liters/hour of air are passed through the fluid. The surface of the fluid is agitated by a gear running at 2540 Rpm. A 4 sq. in. copper catalyst is immersed in the fluid. After 50 hours, viscosity change, acid no., benzene and pentane insolubles are determined. The results for this fluid are:
  • This example illustrates the resistance to mechanical shear of gear lubricants thickened with high viscosity PAO.
  • a 75W-140 gear oil as prepared in Example 1.A.B. was subjected to the Cannon Shear Test. In this test the fluid is subjected to preloaded tapered roller bearings running at 3450 r.p.m. After 8 hrs. under these conditions this fluid lost less than 0.4% of its viscosity.
  • Example 1.A.B. A 75W-140 gear oil as prepared in Example 1.A.B. was used to fill the drive axle of a Class 8 line haul truck. After 30,000 road miles the viscosity was essentially unchanged.
  • This example illustrates the Newtonian character of gear lubricants and engine lubricants thickened with PAO-100.
  • a gear lubricant as prepared in Example 1.B.D. had its viscosity measured at 100°C under no shear conditions (ASTM D-445). The same sample's viscosity was determined at 100°C under a shear rate of 10 6 sec-1 in a Tapered Bearing Simulator and was essentially unchanged.
  • crankcase lubricant as prepared in Example 3.E had its viscosity measured at 150°C under no shear conditions (ASTM D-445). The same sample's viscosity was determined at 150°C under a shear rate of 10 6 sec-1 in a Tapered Bearing Simulator and was essentially unchanged.
  • This example illustrates the oxidative stability of blends of 100 mm 2 /PAO and low viscosity PAO.
  • the low viscosity fluids were 4 and 6 mm 2 /s polydecenes.
  • the blends were stabilized with 0.75 parts per 100 of oil (PHO) of p-nonylphenyl alphanaphthylamine and 0.25 PHO of dilaurylthiodipropionate. They were subjected to a 370°F temperature for 72 hours while air was passed through the solutions at a rate of 5 liters per hour.
  • the oxidation was performed in the presence of Mg, Fe, Cu, AI and Ag metal specimens.
  • the solutions were filtered and the amount of hexane insoluble sludge formed (expressed as mg. per 100 ml.) was determined for each.
  • the results are summarized in the following table.
  • This example illustrates the viscosity index improvement achieved by blending the high viscosity synthetic hydrocarbons (represented by 100 mm 2 /s PAO) and low viscosity synthetic hydrocarbons (represented by 4 and 6 mm 2 /s polydecene) of this invention.
  • This Example (8) also illustrates the feature that VI enhancement is the greatest when the viscosities of the blend components are farthest apart.
  • Example 8 This example is similar to Example 8, but illustrates VI enhancement achieved by blending high viscosity PAO (100 mm 2 /s) with each of two different esters.
  • Example 8 illustrates the VI enhancement shown in Example 8 is valid in ester blends also.
  • the higher VI's of the pure esters contribute to the remarkably high VI's obtained with ester-PAO blends.
  • the high VI's of such blends are manifested in the final lubricants of this invention (as shown in Example 1) and result in extremely good viscosity properties at low temperatures.
  • This example compares directly the oxidative stability of a base fluid thickened with a commercial VI improver (ECA 7480 from Paramin's Division of Exxon) to that of the same base fluid thickened with a high viscosity synthetic hydrocarbon (100 mm 2 /s PAO).
  • the base fluid chosen as the medium to be thickened was a polydecene having KV 210°F of 5.96 mm 2 /s and a VI of 136.
  • the solutions were stabilized with 0.5 PHO of phenyl alphanapthyl amine and 0.25 PHO of dilauryl thiodipropionate.
  • the oxidation test was performed as described in Example 7. A comparison of the solutions before and after testing is summarized in the following table.
  • composition A the polymeric thickener decomposed drastically.
  • the viscosity after testing was nearly equivalent to that of the starting base fluid.
  • the viscosity index of composition A decreased to that of the base fluid, illustrating that oxidation, as well as shear, destroys the V.I. improvement gained by the use of high molecular weight polymeric additives.
  • compositions B. and C. experienced minimal change in viscosity and viscosity index, illustrating the oxidative stability of blends of the high and low viscosity synthetic hydrocarbon of this invention.
  • Ingredients A, B and C represent the thickeners of this invention.
  • Ingredients D and E represent commercial high molecular weight VI improvers.
  • the fluids of this invention (11-A, 11-B and 11-C) can be seen to be far more stable to oxidation than nearly identical fluids prepared using commercial V.I. improvers.
  • the inherent instability of 11-D and 11-E is evidenced by the large changes in viscosity and large decrease in viscosity index suffered by these fluids.
  • the example compares the oxidative stability of a low viscosity fluid thickened with a variety of ethylene-propylene polymers, each having a different viscosity and molecular weight.
  • the low viscosity fluid chosen was a commercial polydecene oligomer having a kinematic viscosity at 100°C (K.V. 100 ) of 3.83 mm 2 /s.
  • K.V. 100 kinematic viscosity at 100°C
  • One hundred ml. of each fluid was heated to 187.8°C for 72 hrs. Air was bubbled through the samples at a rate of 5 liters per hours.
  • Metal washers (Mg, Fe, Ag, Cu, and Al), each having a surface area of 5 cm 2 , were suspended in the fluids as oxidation catalysts and as specimens to determine corrosivity of the oxidized fluids (by weight change). Each sample was protected with exactly the same proprietary antioxidant. Separate studies have shown that the polydecene base fluid is extremely well protected by the antioxidant used. After oxidation, the amount of particulates (sludge) formed was weighed, the acid number of the oils was measured, the viscosity changes of the samples were determined and any weight changes in the metal specimens were measured. A zero change in all these parameters indicates no oxidative degradation. The following tables outline the oils tested and the results of the oxidation test. Where:
  • the thickeners of this invention are much more stable to viscosity and viscosity index losses from oxidation than the current commercial thickener (D).
  • the viscosity losses observed in this test increase as the molecular weight of the thickener increases and decrease when at a given molecular weight, the amount of thickener used decreases.
  • Sample D actually contains only about 2-3% high molecular weight thickener, but the molecular weight is so high relative to A, B and C that its degradation produces much more severe viscosity losses.
  • sample A is quite low molecular weight and so suffers very little change in viscosity despite the large amount of thickener used in its blend.
  • the fluids of this patent having viscosities up to 1000 mm 2 /s at 100°C are shown to have outstanding resistance to oxidative breakdown when compared with currently available thickeners.
  • the relative resistance toward oxidation of the blends is illustrated by the acid developed (measured by acid number) during aging, the particulates (sludge) formed during the test and by weight change of the metal specimens.
  • the following table features data on these parameters.
  • This example illustrates the thickening power and VI, improvement of the oligomers of this invention.
  • One way of comparing thickening power is to ascertain the viscosity increase caused by the addition of a certain percentages of thickener to a common base stock.
  • Thickeners A, B, C and D are ethylene-propylene oligomers of this invention.
  • Thickener.E is LubrizolEJ 7010, a commercial "OCP" thickener consisting of an oil solution of a rubbery high molecular weight ethylene-propylene copolymer.
  • OCP oil solution of a rubbery high molecular weight ethylene-propylene copolymer.
  • the viscosity of Lubrizol 7010 is given as about 1000 mm 2 /s at 100°C.
  • Another way of examining thickeners is to compare how much additive is required to increase the viscosity of a fluid to a given value.
  • the low viscosity polydecene was thickened to 13 mm 2 /s and 24 mm 2 /s with each of the thickeners listed above.
  • fluids of this invention can be so chosen as to require smaller amounts to thicken low viscosity fluids to a given higher viscosity (D vs. E). While thickeners A, B and C require higher treat levels than E, they are surprisingly efficient thickeners for their viscosity and as stated earlier produce a more stable blend.
  • This example describes the preparation of an SAE viscosity grade 10W-40 diesel crankcase oil using a liquid ethylene propylene oligomer having a kinematic viscosity at 100°C of 432 mm 2 /s.
  • the lubricant has the following properties-
  • This example describes the preparation of an SAE viscosity grade 75W-140 automotive gear oil using a liquid ethylene propylene oligomer having a kinematic viscosity at 100°C of 432 mm 2 /s.
  • the lubricant has the properties shown:
  • This example describes the preparation of an SAE viscosity grade 10W-40 diesel crankcase lubricant using an ethylene propylene oligomer having a kinematic viscosity at 100°C of 945 mm l /s.
  • the lubricant has the properties shown:
  • This example illustrates the preparation of an automotive gear lubricant SAE viscosity grade 75W-140 using a liquid ethylene-propylene oligomer having a kinematic viscosity at 100°C of 265 mm 2 /s.
  • the lubricant has the properties shown:
  • This example illustrates the preparation of a diesel crankcase lubricant SAE viscosity grade 10W-40 using a liquid ethylene-propylene oligmer having a kinematic viscosity at 100°C of 945 mm 2 /s.
  • the lubricant has the properties shown:
  • This example illustrates the preparation of an ISO VG 460 industrial gear lubricant from an ethylene-propylene oligomer having a kinematic viscosity at 100°C of 945 mm 2 /s.
  • the lubricant has the properties shown:
  • This example compares the oxidative stability of fully formulated crankcase oil utilizing the hydrogenated polyisoprenes of this invention with essentially identical formulations thickened to the same viscosity with two commercially available high molecular weight ethylene-propylene rubber based thickeners and a purchased sample of high quality crankcase oil.
  • One hundred ml. of each fluid was heated to 187.8°C for 72 hrs. Air was bubbled through the samples at a rate of 5 liters per hour.
  • Metal washers Mg, Fe, Cu and Al
  • Each sample contained a low viscosity polydecene and equal amounts of ester and additive package. After oxidation, the changes in viscosity and viscosity index were determined as well as the weight changes in the metal specimens. The following tables outline the formulations and their unaged viscometrics as well as the changes wrought by oxidation.
  • the low viscosity synthetic hydrocarbon (SHC) in the blends was a polydecene having a K.V.100°c of 3.83 mm 2 /s.
  • the ester was di-2-ethylhexyl azelate and the package was Lubrizol @ 4856.
  • composition of the present invention (A), is superior in oxidative stability to prior art B, C and D. As can be seen, composition A suffered no loss in viscosity and minimal change in viscosity index. These features predict much greater "stay-in-grade" performance for the compositions of this invention.
  • composition A was found to produce less corrosion to Cu and Ag than the other compositions.
  • the following table outlines the weight change observed (in mg/cm 2 ) in the Cu and Ag metal specimens for the tested formulations.
  • This example compares the thickening power of the hydrogenated polyisoprene oligomers of this invention with a commercial "OCP” thickener, Lubrizol® 7010, which is a solution of high molecular weight ethylene-propylene rubber in oil. Solutions made by dissolving varying amounts of different thickeners in a low viscosity (3.83 mm 2 /s at 100°C) polydecene. The dependence of thickening power on viscosity of the thickener is clearly seen.
  • the thickening power of A, B, C and D (the oligomers of this invention) is seen to correlate with the viscosity of the oligomer.
  • Thickener E having a viscosity of about 1000 mm 2 /s at 100°C (greater than even E of the invention) is not as effective in increasing viscosity of the base fluid as are the higher viscosity fluids of the invention. This finding is unexpected.
  • the hydrogenated polyisoprene oligomers (HPO) of this invention act as viscosity index improvers.
  • the following data show the viscosity index of a low viscosity polydecene (3.83 mm 2 /s) after thickening to 24 mm 2 /s with A, B, C and D.
  • This example illustrates the preparation of an SAE viscosity grade 75W-140 automotive gear lubricant using a hydrogenated polyisoprene oligomer of 245 mm 2 /s at 100°C.
  • the lubricant had the following properties:
  • This example illustrates the preparation of an SAE viscosity grade 10W-40 diesel crankcase lubricant from a hydrogenated polyisoprene with a kinematic viscosity of 245 mm 2 /s at 100°C.
  • the lubricant had the following properties:
  • This example illustrates the preparation of SAE viscosity grade 10W-40 diesel crankcase oils using hydrogenated polyisoprene oligomers having the kinematic viscosities at 100°C shown.
  • the lubricants had the properties shown:
  • This example illustrates the preparation of an SAE viscosity grade 75W-140 automotive gear lubricant using hydrogenated polyisoprene oligomers having the kinematic viscosities at 100°C shown.
  • the lubricants had the properties shown:
  • This example describes the preparation of an SAE 10W-40 diesel crankcase lubricant using a hydrogenated polyisoprene oligomer having a kinematic viscosity of 245 mm 2 /s at 100°C.
  • This example illustrates the preparation of an SAE viscosity grade 75W-140 automotive gear oil using a hydrogenated polyisoprene oligomer having a kinematic viscosity at 100°C of 245 mm 2 /s.
  • the lubricant had the following properties:

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Claims (7)

1. Schmiermittelzusammensetzung, die
(A) ein Poly-alpha-olefin mit einer Viskosität von 40 bis 1000 mm2/s bei 100°C,
(B) einen synthetischen Kohlenwasserstoff mit einer Viskosität von 1 bis 10 mm2/s bei 100°C,
(C) einen Ester mit einer Viskosität von 1 bis 10 mm2/s bei 100°C und
(D) ein Zusatzmittelpaket mit mindestens einem Zusatzmittel, das aus der Gruppe ausgewählt ist, die im wesentlichen aus Dispergiermitteln, Oxidationsverhinderen, Korrosionsschutzmitteln, Verschleißschutzmitteln, Fließpunktserniedrigern, Rostverhütungsmitteln, Antischaummitteln und Hochdruckzusätzen besteht, enthält.
2. Schmiermittelzusammensetzung, die
(A) ein Ethylen-alpha-Olefin-Oligomer mit einer Viskosität von 40 bis 1000 mm2/s bei 100°C und
(B) einen synthetischen Kohlenwasserstoff mit einer Viskosität von 1 bis 10 mm2/s bei 100°C enthält.
3. Zusammensetzung nach Anspruch 2, die ferner einen Ester mit einer Viskosität von 1 bis 10 mm2/s bei 100°C enthält.
4. Schmiermittelzusammensetzung, die
(A) ein hydriertes Polyisopren-Oligomer mit einer Viskosität von 40 bis 1000 mm2/s bei 100°C und
(B) einen synthetischen Kohlenwasserstoff mit einer Viskosität von 1 bis 10 mm2/s bei 100°C enthält.
5. Zusammensetzung nach Anspruch 4, die ferner einen Ester mit einer Viskosität von 1 bis 10 mm2/s bei 100°C enthält.
6. Schmiermittelzusammensetzung, die
(A) ein hydriertes Polyisopren-Oligomer mit einer Viskosität von 40 bis 1000 mm2/s bei 100°C und
(B) einen Ester mit einer Viskosität von 1 bis 10 mm2/s bei 100°C enthält.
7. Schmiermittelzusammensetzung nach Anspruch 2 bis 6, die ferner ein Zusatzmittelpaket mit mindestens einem Zusatzmittel, das aus der Gruppe ausgewählt ist, die im wesentlichen aus Dispergiermitteln, Oxidationsverhinderern, Korrosionsschutzmitteln, Verschleißschutzmitteln, Fließpünktserniedrigern, Rostverhütungsmitteln, Antischaummitteln und Hochdruckzusätzen besteht, enthält.
EP83102377A 1982-03-10 1983-03-10 Schmiermittelzusammensetzung Expired EP0088453B1 (de)

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