EP0638632B1 - Motorölzusammensetzungen, Zusatzkonzentrat zur Herstellung solcher Öle und ihre Verwendung - Google Patents

Motorölzusammensetzungen, Zusatzkonzentrat zur Herstellung solcher Öle und ihre Verwendung Download PDF

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Publication number
EP0638632B1
EP0638632B1 EP94305974A EP94305974A EP0638632B1 EP 0638632 B1 EP0638632 B1 EP 0638632B1 EP 94305974 A EP94305974 A EP 94305974A EP 94305974 A EP94305974 A EP 94305974A EP 0638632 B1 EP0638632 B1 EP 0638632B1
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Prior art keywords
calcium
tbn
oil
overbased
per gram
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EP94305974A
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English (en)
French (fr)
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EP0638632A3 (de
EP0638632A2 (de
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Susan M. Nicholson
Roger Scattergood
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Afton Chemical Ltd
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Afton Chemical Ltd
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    • C10N2040/28—Rotary engines

Definitions

  • This invention relates to lubricant compositions, and more particularly to lubricants and additive concentrates of enhanced performance characteristics.
  • An objective therefore is to provide novel compositions capable of effectively controlling wear and formation of undesirable quantities of such varnish, sludge, and carbonaceous deposits.
  • U.S. Pat. No. 5,080,815 to Fenoglio et al describes dispersants having improved compatibility toward a particular fluoroelastomer. Those dispersants are formed by reacting a hydrocarbyl-substituted dicarboxylic acid compound such as a hydrocarbyl-substituted dicarboxylic acid anhydride with aminoguanidine or a basic salt thereof in a ratio of about 1.5 to about 2.2 moles of aminoguanidine or basic salt thereof per mole of hydrocarbyl-substituted dicarboxylic acid compound.
  • a hydrocarbyl-substituted dicarboxylic acid compound such as a hydrocarbyl-substituted dicarboxylic acid anhydride
  • aminoguanidine or a basic salt thereof in a ratio of about 1.5 to about 2.2 moles of aminoguanidine or basic salt thereof per mole of hydrocarbyl-substituted dicarboxylic acid compound.
  • U.S. Pat. No. 4,908,145 to Fenoglio describes dispersants for lubricating oils that are also compatible with that fluorohydrocarbon elastomer. These dispersants are enriched in alkyl-bis-3-amino-1,2,4-triazole (e.g., polybutenyl-bis-3-amino-1,3,4-triazoles) and are formed by reacting an alkyl-substituted dicarboxylic acid compound, such as a polyisobutenyl succinic acid compound, with a basic salt of aminoguanidine at a ratio of from about 1.6 to about 2 moles of aminoguanidine compound per mole of the alkyl-substituted dicarboxylic acid compound.
  • alkyl-bis-3-amino-1,2,4-triazole e.g., polybutenyl-bis-3-amino-1,3,4-triazoles
  • this invention provides a lubricant composition which comprises a major amount of oil of lubricating viscosity containing at least the following components:
  • the lubricant composition further comprises up to 0.1 wt% of magnesium as an overbased magnesium detergent additive complement having a TBN of at least 300 mg of KOH per gram.
  • the lubricant composition further comprises at least one oil-soluble antioxidant and at least one foam inhibitor, and/or at least one viscosity index improver.
  • the lubricant compositions have a TBN in the range of 6 to 15 mg of KOH per gram.
  • Preferred zinc dihydrocarbyl dithiophosphates are mixtures of zinc dialkyl dithiophosphates containing primary and secondary alkyl groups and in which at least 35 mol % of the alkyl groups are secondary alkyl groups.
  • the basic calcium detergent additive complement in the compositions of this invention is comprised of a mixture of (i) and (ii), or (i) and (iii), or (i), (ii) and (iii), wherein (i) is an overbased calcium sulfonate detergent composition having a TBN of at least 280 mg of KOH per gram thereof, and is present in amount such that at least 40 wt% of the calcium is derived therefrom; (ii) is an overbased calcium sulfurized phenate detergent composition having a TBN of at least 100 mg, preferably at least 200 mg, of KOH per gram thereof, and if present is present in amount such that up to 50 wt% of the calcium is derived therefrom; and (iii) is a low base calcium sulfonate detergent having a TBN of up to 40 mg of KOH per gram thereof, and if present is present in amount such that up to 25 wt% of the calcium is derived therefrom.
  • At least 50 wt% of the magnesium of the overbased magnesium detergent additive complement is comprised of an overbased magnesium sulfonate detergent composition having a TBN of at least 300 mg of KOH per gram thereof.
  • Preferred oil-soluble dispersant products used pursuant to this invention are formed by reacting aminoguanidine and/or a basic salt thereof with an alkenyl succinic acylating agent in a mol ratio in the range of 0.8 to 1.2 mols of aminoguanidine and/or basic salt thereof per mole of the acylating agent.
  • the alkenyl group of the acylating agent is derived from a polyolefin having a GPC number average molecular weight in the range of 900 to 2500.
  • additive concentrates which comprise at least the following components:
  • these additive concentrates have a TBN in the range of 50 to 120 mg KOH per gram.
  • additive components such as described above can be used in formulating motor oil compositions that can pass at least the following tests:
  • the base oils used in forming the lubricant compositions of this invention can be natural or synthetic oils of lubricating viscosity, or suitable blends thereof.
  • the base oils can be hydrocarbon oils derived from petroleum (or tar sands, coal, shale, etc.).
  • the base oils can be or include natural oils of suitable viscosities such as rapeseed oil, etc., and synthetic oils such as hydrogenated polyolefin oils; poly- ⁇ -olefins (e.g., hydrogenated or unhydrogenated ⁇ -olefin oligomers such as hydrogenated poly-1-decene); alkyl esters of dicarboxylic acids; complex esters of dicarboxylic acid, polyglycol and alcohol; and the like. Mixtures of mineral, natural and/or synthetic oils in any suitable proportions are also useable.
  • natural oils of suitable viscosities such as rapeseed oil, etc.
  • synthetic oils such as hydrogenated polyolefin oils; poly- ⁇ -olefins (e.g., hydrogenated or unhydrogenated ⁇ -olefin oligomers such as hydrogenated poly-1-decene); alkyl esters of dicarboxylic acids; complex esters of dicarboxylic acid, polyglycol and alcohol;
  • the base oil is preferably a petroleum-derived mineral oil of the types conventionally used in forming passenger car, heavy duty diesel engine oils, or drivetrain lubricants.
  • AG dispersant is used to designate a product made by reacting aminoguanidine or a basic salt thereof with a hydrocarbyl-substituted succinic acid or anhydride in a mole ratio of from about 0.4 to 1.3 moles of the aminoguanidine or basic salt thereof per mole of the succinic acid or anhydride compound.
  • borated AG dispersant is used to designate a product made in two stages, namely, (i) reacting aminoguanidine or a basic salt thereof with a hydrocarbyl-substituted succinic acid or anhydride in a mole ratio of from about 0.4 to 1.3 moles of the aminoguanidine or basic salt thereof per mole of the succinic acid or anhydride compound; and (ii) borating the product so produced.
  • a suitably proportioned mixture of an aliphatic hydrocarbyl-substituted succinic acid derivative (acid, anhydride, lower alkyl ester, or acyl halide) and aminoguanidine or a basic salt thereof is heated, preferably under an inert atmosphere, at a temperature in the range of about 120 to about 200°C.
  • an inert atmosphere such as a light mineral oil. Reaction times are typically in the range of from 1 to 4 hours.
  • Suitable inert atmospheres include nitrogen, argon, krypton, neon, etc.
  • AG dispersants are characterized by having a peak in the region of 1590 cm -1 . Additionally, the spectrum may exhibit a peak in the range of 1690 cm -1 , but AG dispersants can be used that do not exhibit this latter peak. When made at mol ratios of about 1:1 or lower, a peak at 1725 cm -1 appears. The 1590 cm -1 peak is nearly absent in the Examples of U.S. Pat. No. 5,080,815.
  • the chemical structure of the products of this invention is unknown, but on the basis of their infrared spectra, they do not appear to have any significant content of triazole moieties, as is shown by the absence of the 1640 cm -1 IR peak present in the Examples of U.S. Pat. No. 5,080,815.
  • Example 1 The procedure of Example 1 is repeated using a chemically equivalent amount of PSA formed from polyisobutylene having a number average molecular weight of about 1290 in lieu of the higher molecular weight PSA of Example 1.
  • Example 1 The procedure of Example 1 is repeated except that the AGB:PSA mole ratio is 1.1:1.
  • Example 3 is repeated except that the PSA of Example 2 is employed.
  • Product formed as in Example 3 is borated by heating 2290 g of the 44% active product so formed with 212.5 g of a superborated polyisobutenyl succinic ester-amide containing approximately 2.5% of boron at 160°C for 2 hours.
  • the resultant product is diluted with 154 g oil to give a product containing 0.2% boron.
  • Example 5 is repeated, but using 2000 g of product formed as in Example 4 and 185.6 g of the superborated ester-amide.
  • the boron content of the borated product is 0.2% on dilution with 134 g oil.
  • Example 7 is repeated with the exception that 2000 g of active product formed as in Example 2 is used instead of the higher molecular weight product of Example 1.
  • Example 1 The procedure of Example 1 is repeated seven times in the same manner except that the proportions of AGB and PSA are varied such that the respective AGB:PSA mole ratios are 0.4:1, 0.5:1. 0.6:1, 0.7:1, 1.0:1, 0.9:1 and 1:1.
  • Examples 9-15 are repeated, but using product formed as in Example 2 in place of the product formed as in Example 1.
  • Example 1 is repeated except that 1.0 mole of AGB is reacted with 1.0 mole of PSA. Boration is carried out as described in Example 5 to provide a preferred product of this invention.
  • Component b It is important to use an oil-soluble zinc dihydrocarbyl dithiophosphate in which at least 35 mol % of the hydrocarbyl groups present are secondary hydrocarbyl groups, such as isopropyl, sec-butyl, and/or 4-methyl-2-pentyl groups.
  • an oil-soluble zinc dihydrocarbyl dithiophosphate in which at least 35 mol % of the hydrocarbyl groups present are secondary hydrocarbyl groups, such as isopropyl, sec-butyl, and/or 4-methyl-2-pentyl groups.
  • a mixture of zinc dihydrocarbyl dithiophosphates is employed.
  • One way of achieving such mixtures is to combine appropriate proportions of an all-primary zinc dialkyl dithiophosphate with an all-secondary zinc dialkyl dithiophosphate.
  • the dithiophosphoric acids from which the zinc salts are formed can be prepared by the reaction of about 4 moles of one or more alcohols per mole of phosphorus pentasulfide, and the reaction may be carried out within a temperature range of from about 50 to about 120°C. The reaction generally is completed in about 1 to 10 hours. Hydrogen sulfide is liberated during the reaction.
  • Primary alcohols which may be used in forming the dialkyl dithiophosphoric acid intermediate include propanol, butanol, isobutyl alcohol, pentanol, neopentanol, hexanol, heptanol, 2-ethyl-1-hexanol, isooctyl alcohol, nonanol, decanol, undecanol, dodecanol, tridecanol, tetradecanol, octadecanol, eicosanol, and the like.
  • each alkyl group in the dithiophosphoric acid intermediate typically contains in the range of 3 to about 20 carbon atoms, preferably in the range of 3 to about 12, and most preferably in the range of 3 to about 8 carbon atoms.
  • the preparation of the zinc salts of the dialkyl dithiophosphoric acid intermediates is usually effected by reacting the acid product with a suitable zinc compound such as zinc oxide or zinc hydroxide. Simply mixing and heating such reactants is normally sufficient to cause the reaction to occur, and the resulting product is usually of sufficient purity for use without further purification.
  • the salts are formed in the presence of a diluent such as an alcohol, water or a light mineral oil.
  • Neutral salts are prepared by reacting one equivalent of zinc oxide or hydroxide with one equivalent of the acid.
  • Basic metal salts are prepared by adding an excess (i.e., more than one equivalent) of the metal oxide or hydroxide with one equivalent of the dialkyl dithiophosphoric acid. Typical procedures for producing zinc dialkyl dithiophosphates are given in U.S. Pat. Nos. 4,085,053; 4,104,291; 4,215,067; and 4,634,541.
  • incorporation of certain ingredients such as small amounts of metal acetate or acetic acid in conjunction with the zinc reactant will facilitate the reaction and provide an improved product.
  • certain ingredients such as small amounts of metal acetate or acetic acid
  • use of up to about 5% of zinc acetate in combination with the required amount of zinc oxide tends to facilitate the formation of zinc dialkyl dithiophosphates.
  • one or more of the zinc dialkyl dithiophosphates may be treated with an epoxide (e.g., an alkylene oxide having up to about 8 carbon atoms in the molecule) to form an adduct.
  • an epoxide e.g., an alkylene oxide having up to about 8 carbon atoms in the molecule
  • zinc salts is a mixture of dialkyl dithiophosphates wherein the zinc salts contain from about 4.8 to about 6.6% by weight of isobutyl groups, from about 4.8 to about 6.7% by weight of 2-ethyl-1-hexyl groups, from about 14.0 to about 14.5% by weight of isopropyl groups, and from about 16.7 to about 20.1% by weight of 4-methyl-2-pentyl groups.
  • Another particularly preferred mixture of zinc dialkyl dithiophosphates is a mixture which contains from about 4.6 to about 6.4% by weight of isobutyl groups, from about 2.2 to about 3.1% by weight of primary amyl groups, from about 1.4 to about 2.0% by weight of primary octyl groups, from about 11.6 to about 12.7% by weight of isopropyl groups, and from about 21.4 to about 23.4% by weight of 4-methyl-2-pentyl groups.
  • the weight percentages of the respective alkyl groups as set forth in this paragraph are based on the total weight of the zinc salts which, for the purposes of calculation only, are assumed to have the general formula: where each R is one of the designated alkyl groups.
  • the amount of any solvent or diluent that may be present in the mixture of zinc dialkyl dithiophosphates is omitted, and the assumption is made --solely for the purposes of the calculations -- that the zinc dialkyl dithiophosphates are not overbased, or treated with an epoxide or zinc carboxylate, although in fact they may be overbased and/or treated in such manner.
  • One way of forming a typical mixture of zinc salts characterized by having on a weight basis about 4.8 to about 6.6% by weight of isobutyl groups, from about 4.8 to about 6.7% by weight of 2-ethyl-1-hexyl groups, from about 14.0 to about 14.5% by weight of isopropyl groups, and from about 16.7 to about 20.1% by weight of 4-methyl-2-pentyl groups is to mix LUBRIZOL® 1060 zinc dialkyldithiophosphate and HiTEC® 685 zinc dialkyldithiophosphate in a weight ratio (using both additives on an as received basis) of 1.79:1, respectively.
  • one way of forming a typical mixture of zinc salts having on a weight basis from about 4.6 to about 6.4% by weight of isobutyl groups, from about 2.2 to about 3.1% by weight of primary amyl groups, from about 1.4 to about 2.0% by weight of primary octyl groups, from about 11.6 to about 12.7% by weight of isopropyl groups, and from about 21.4 to about 23.4% by weight of 4-methyl-2-pentyl groups is to mix HiTEC® 7169 zinc dialkyldithiophosphate and either HiTEC® 7198 or 7197 zinc dialkyldithiophosphate in a weight ratio (again, both additives being weighed on an as received basis) of 3.29:1, respectively.
  • LUBRIZOL is a trademark of The Lubrizol Corporation and HiTEC is a trademark of Ethyl Petroleum Additives, Ltd.,and Ethyl Petroleum Additives, Inc.
  • Component c) comprises one or more calcium salts of at least one acidic organic compound. These include low-based and overbased calcium sulfonates, low-base and overbased calcium phenates, low-base and overbased calcium sulfurized phenates, and low-base and overbased calcium carboxylates.
  • overbased is used to designate metal salts wherein the metal is present in stoichiometrically larger amounts than the organic acid radical. Thus this term is inclusive of those material which have been referred to in the art as overbased, superbased, hyperbased, etc.
  • overbased calcium salts useful in this invention contain from about 1.1 to about 40 or more equivalents of calcium, more preferably from about 1.5 to about 30 and most preferably from about 2 to about 25 equivalents of calcium for each equivalent of material which is overbased.
  • overbased materials are prepared by treating with an acidic material, a reaction mixture comprising the organic material to be overbased, a reaction medium consisting essentially of at least one inert, organic solvent for the organic material to be overbased, a stoichiometric excess of a metal base, and a promoter.
  • the most commonly employed methods involve use of a mineral oil as the reaction medium and a stoichiometric excess of metal oxide, hydroxide, alkoxide, carbonate, bicarbonate, or sulfide as the metal base.
  • Suitable acidic materials used in producing the overbased salts include such acids as formic acid, acetic acid, oleic acid, palmitic acid, nitric acid, sulfuric acid, hydrochloric acid, hydrobromic acid, carbamic acid, substituted carbamic acids, boric acid, SO 2 , SO 3 , CO 2 , H 2 S, N 2 O 3 , and the like.
  • the most preferred acid material for use in forming the overbased calcium salts is carbon dioxide.
  • Examples of compounds useful as the promoter include phenolic substances such as phenol, naphthol, alkylphenol, thiophenol, sulfurized alkylphenol, and condensation products of formaldehyde with a phenolic substance; alcohols such as methanol, ethanol.
  • reaction mass is filtered on completion of the overbasing operation.
  • suitable promoters see U.S. Pat. Nos. 2,616,904; 2,695,910 and 2,777,874.
  • a particularly effective method for preparing the overbased calcium salts comprises mixing an acid with an excess of a basic calcium neutralizing agent such as calcium oxide or hydroxide and at least one alcohol promoter, and carbonating the mixture at an elevated temperature such as 60° to 300°C, and preferably about 100 to about 200°C.
  • a basic calcium neutralizing agent such as calcium oxide or hydroxide and at least one alcohol promoter
  • the overbased calcium salts can also be formed by overbasing a preformed low base or non-overbased calcium salt.
  • the overbased calcium sulfonates can be derived from suitable aliphatic, cycloaliphatic, aromatic or heterocyclic sulfonic acids and/or the salts thereof.
  • such acids can be represented by the formulas R(SO 3 H) n and (R') x T(SO 3 H) y where R is an aliphatic or aliphatic-substituted cycloaliphatic group free from acetylenic unsaturation and having up to about 60 carbon atoms; n is at least one, and is generally in the range of 1 to 3; R' is an aliphatic group free from acetylenic unsaturation (typically alkyl or alkenyl) and having about 4 to about 60 carbon atoms; T is a cyclic nucleus which may be derived from an aromatic hydrocarbon such as benzene, toluene, xylene, naphthalene, anthracene, biphenyl, etc., or from a
  • T is an aromatic hydrocarbon nucleus such as benzene or naphthalene; and x and y have an average value of about 1 to 4 per molecule, most often an average of about 1.
  • acids are petroleum sulfonic acids, paraffin wax sulfonic acids, wax-substituted cyclohexyl sulfonic acids, cetylcyclopentyl sulfonic acids, wax-substituted aromatic sulfonic acids, mahogany sulfonic acids, tetraisobutylene sulfonic acids, tetraamylene sulfonic acids, and the like.
  • the overbased calcium salts are formed from alkylaryl sulfonic acids, such as alkylbenzene sulfonic acids.
  • alkyl group or groups present on the aromatic ring typically each contain from about 8 to about 40 carbon atoms.
  • Suitable overbased calcium sulfonates having total base numbers of at least about 150 milligrams of KOH per gram of the overbased composition are available as articles of commerce from a number of well known suppliers.
  • HiTEC® 611 additive Ethyl Petroleum Additives, Inc.
  • Overbased calcium phenates are typically formed by overbasing calcium alkylphenates and/or calcium alkenylphenates where the aromatic ring is substituted with one or more alkyl or alkenyl groups (usually 1 to 2) that render the finished product soluble or at least stably dispersible in oil.
  • the alkyl or alkenyl substituents on the aromatic ring typically contain at least about 6 carbon atoms and may contain as many as 500 or more carbon atoms.
  • Preferred substituents are derived from alpha-olefins such as are formed by wax cracking or chain growth of ethylene on aluminum alkyls such as triethyl aluminum, or from olefin oligomers such as olefin dimers, trimers, tetramers and/or pentamers.
  • alpha-olefins such as are formed by wax cracking or chain growth of ethylene on aluminum alkyls such as triethyl aluminum, or from olefin oligomers such as olefin dimers, trimers, tetramers and/or pentamers.
  • higher polymers such as polypropenes, polyisobutenes, polyamylenes, and copolymers such as copolymers of ethylene and propylene, etc., are also useful as source materials for forming the substituted phenols from which the calcium phenate is produced.
  • the phenate will have an alkyl or alkenyl substituent having in
  • the phenolic ring may also additionally contain short chain substituents such as methyl, ethyl, isopropyl, butyl, etc. substituents.
  • the phenate may be a derivative of a polyhydroxy aromatic compound, such as catechol, resorcinol, or hydroquinone.
  • the overbased sulfurized calcium phenates can be formed from the substituted phenols described above by reacting the substituted phenol with sulfur monochloride, sulfur dichloride or elemental sulfur.
  • the phenol:sulfur compound molar ratio is usually in the range of about 1:0.5 to about 1:1.5 or more. Reaction temperatures in the range of about 60 to about 200°C are usually employed. Generally the phenol:sulfur group molar ratio in the sulfurized phenate is in the range of about 2:1 to about 1:2.
  • the overall process for producing the overbased sulfurized calcium phenate can be conducted in multiple stages as by forming the sulfurized phenol and then conducting the overbasing process which itself can be operated in stages with multiple introduction of additional reactants, promoters, etc.
  • the sulfurization and overbasing can be conducted concurrently by charging the reactants such that the sulfurized phenol or phenate is formed in situ and is overbased as the reaction proceeds. All such process details are well known and reported in the literature.
  • Suitable overbased carboxylic acids which can be used in this invention include overbased aliphatic carboxylic acids, overbased cycloaliphatic carboxylic acids, overbased aromatic carboxylic acids, and overbased heterocyclic carboxylic acids.
  • Such acids can be monocarboxylic or polycarboxylic acids, and the principal requirement is that the acid have sufficient chain length to be soluble or at least stably dispersible in lubricating oil.
  • the acids generally contain from about 8 to about 50, and preferably from about 12 to about 30, carbon atoms, although certain acids such as alkyl- or alkenyl-substituted succinic acids can have an average of up to 500 or more carbon atoms per molecule.
  • the acids are usually free of acetylenic unsaturation.
  • Examples include linolenic acid, capric acid, linoleic acid, oleic acid, stearic acid, lauric acid, ricinoleic acid, undecylic acid, palmitoleic acid, 2-ethylhexanoic acid, myristic acid, isostearic acid, behenic acid, pelargonic acid, propylene tetramer-substituted succinic acid, isobutene trimer-substituted succinic acid, octylcyclopentane carboxylic acid, stearyl-octahydroindenecarboxylic acid, tall oil acids, rosin acids, polybutenyl succinic acids derived from polybutene having a GPC number average molecular weight in the range of 200 to 1500, acids formed by oxidation of wax, and like acids.
  • the preferred overbased carboxylic acids are the overbased aromatic carboxylic acids in which the aromatic nucleus is substituted by at least one carboxyl group (usually 1 to 4, preferably 1 to 2) and by at least one aliphatic hydrocarbyl group (usually 1 to 2, preferably one), preferably derived from a polyalkene, and most preferably having an average in the range of about 40 to about 400 carbon atoms.
  • the aromatic nucleus is also substituted by at least one hydroxyl group (usually 1 to 2, preferably one).
  • substituted aromatic carboxylic acids include substituted benzoic, phthalic, and salicylic acids.
  • aromatic carboxylic acids are the overbased calcium salts of aliphatic-substituted salicylic acids wherein the substituent is derived from polyalkenes, particularly polymerized lower 1-monoolefins, such as polyethylene, polypropylene, polyisobutylene, ethylene-propylene copolymers, etc., having average carbon contents of about 50 to about 400 carbon atoms.
  • Overbased calcium calixerates such as described in U.S. Pat. No. 5,114,601 are also suitable.
  • Suitable low base calcium alkylbenzene sulfonate detergent compositions are formed by preparing an alkali or alkaline earth metal salt of an alkylbenzene sulfonic acid and if desired, subjecting the salt in the presence of a small excess of an alkali or alkaline earth metal base such as an oxide, hydroxide or alcoholate to the action of an acidic material such as carbon dioxide so that a small amount of overbasing occurs.
  • This controlled overbasing can be conducted using the same materials in much the same way as the overbasing described above, except of course the amount of metal base is such that the desired total base number of the resultant composition is achieved.
  • Suitable low base materials of the foregoing types are available as articles of commerce.
  • HiTEC® 614 additive (Ethyl Petroleum Additives, Inc.) is a good example of a commercially-available calcium alkylbenzene sulfonate.
  • Low-base calcium sulfurized alkylphenates are also suitable components in the compositions of this invention.
  • the overbased magnesium salts utilized pursuant to this invention are generally similar in character to the overbased calcium salts.
  • the overbased magnesium salts are overbased magnesium salts of at least one acidic organic compound, and thus include overbased magnesium sulfonates, overbased magnesium phenates, overbased magnesium sulfurized phenates, overbased magnesium carboxylates, and overbased magnesium calixerates.
  • the processes by which overbased magnesium salts are produced are in many respects similar to the processes used in forming the overbased calcium salts. However, despite these similarities it is desirable pursuant to this invention to utilize a combination of at least one overbased calcium salt and at least one overbased magnesium salt.
  • overbased magnesium salts can be utilized for producing the overbased magnesium salts.
  • Desirable processes for producing overbased magnesium sulfonates are described for example in U.S. Pat. Nos. 4,137,186; 4,201,682; and 4,474,710.
  • Other suitable overbased magnesium salts and/or other methods for producing suitable overbased magnesium salts are described for example in U.S. Pat. Nos. 4,647,387; 4,775,490; 4,957,642; 5,032,299; 5,089,155; and 5,173,203.
  • Synthesis of overbased magnesium calixerates is described in U.S. Pat. No. 5,114,601.
  • a variety of suitable overbased magnesium salts are available as articles of commerce from a number of different suppliers.
  • the preferred overbased magnesium salts are overbased magnesium alkylbenzene sulfonate detergent compositions having a total base number of at least about 300 milligrams of KOH per gram thereof, and most preferably a total base number ber in the range of about 350 to about 500 milligrams of KOH per gram thereof. Since such compositions are formed in an inert diluent, usually a mineral oil diluent, the total base number reflects the basicity of the overall composition including diluent, and any other materials (e.g., promoter, etc.) that may be contained in the detergent composition.
  • compositions of this invention can be used in the compositions of this invention.
  • additives include alkali metal detergents, oxidation inhibitors, friction modifiers, rust inhibitors, foam inhibitors, copper corrosion inhibitors, demulsifying agents, and the like.
  • Alkali metal detergents include sodium, potassium and lithium alkylbenzene sulfonates and sulfurized alkyl phenates.
  • Oxidation inhibitors include phenolic antioxidants, amine antioxidants, organic copper compounds, organo borates, organo phosphites, organo phosphates, organo thio- or dithiophosphates, and the like.
  • phenolic antioxidants include alkylated monophenols, alkylated hydroquinones, sulfur-bridged alkylphenols, methylene-bridged alkylphenols, and hydroxybenzyl-substituted aromatic compounds.
  • Amine antioxidants include phenylene diamines, amino diphenylamines, phenyl-substituted naphthalenes, alkyl-substituted aromatic secondary amines, aminophenols, and the like.
  • the finished lubricants of the invention may contain pour point depressants, materials which are used in oil-base compositions to improve low temperature properties. See, for example, the books Lubricant Additives by C. V. Smalheer and R. Kennedy Smith (Lezius-Hiles Co. Publishers, Cleveland, Ohio, 1967); Gear and Transmission Lubricants by C. T. Boner (Reinhold Publishing Corp., New York, 1964); and Lubricant Additives by M. W. Ranney (Noyes Data Corporation, New Jersey, 1973) for discussions of this subject.
  • additives can be used in the practice of this invention as long as they are compatible with the remainder of the composition and do not materially interfere with the performance of the composition.
  • the ancillary components utilized in the finished lubricants of this invention are typically employed in the following weight percentages based on the weight of the finished lubricant composition:
  • Ancillary Components General Range Preferred Range Oxidation Inhibitor 0 - 4 0.05 - 2 Friction Modifier 0 - 3 0 - 1 Rust Inhibitor 0 - 3 0.02 - 1 Foam Inhibitor 0 - 0.3 0.0002 - 0.1 Copper Corrosion Inhibitor 0 - 0.3 0 - 0.1 Demulsifying Agent 0 - 0.1 0 - 0.02 Viscosity Index Improver 0 - 15 0 - 12 Pour Point Depressant 0 - 5 0 - 2 Supplemental ashless dispersant 0 - 5 0 - 10
  • the additive concentrates of this invention will contain the various ingredients in amounts proportioned to yield finished lubricants having the proportions of the respective ingredients as set forth above.
  • the additive concentrates will contain less than 50 weight %, e.g., a total of from 2 to 45 weight %, of diluents or solvents such as light mineral oil with the balance of the composition being composed of the respective additives being utilized.
  • the following additive components are blended into a base oil blend of 150 and 600 solvent neutral mineral oils: 7.0% of AG dispersant, 1.0% of zinc di-(secondary alkyl)dithiophosphate wherein the alkyl groups are isopropyl and 4-methyl-2-pentyl groups (HiTEC® 7169 additive; Ethyl Petroleum Additives Ltd.; Ethyl Petroleum Additives, Inc.), 0.3% of mixed primary and secondary alkyl zinc dialkyl dithiophosphate (HiTEC® 1656 additive), 1.3% of overbased calcium alkylbenzene sulfonate having a nominal TBN of 300 (HiTEC® 611 additive), 0.9% of low-base calcium alkylbenzene sulfonate having a nominal TBN of 20 (HiTEC® 7304 additive), 1.5% of overbased calcium sulphurized alkylphenate having a nominal TBN of 255, 0.4% of overbased magnesium alkylbenzene sulfonate having a nominal TBN of 400, 0.5% of
  • the AG dispersant is formed from aminoguanidine bicarbonate and polyisobutenyl succinic anhydride derived from polyisobutene having a GPC number average molecular weight of about 2100. These are reacted in a mol ratio of approximately 1:1, and the product is post-borated to a level of 0.2% boron.
  • the lubricant is formulated to 15W40 grade using TLA 347E viscosity index improver (Texaco Chemical Co.). Motor oil formulated in this manner and having a TBN of 11.0 was subjected to the following qualification test procedures:
  • a finished 15W40 engine oil is produced as in Example I except that the antioxidant system used is composed of 0.6% of methylene-bridged alkyl phenol antioxidant (HiTEC® 4782 additive), 0.2% of tertiary butyl phenol antioxidant (HiTEC® 4733 additive), and 0.25% of the Naugalube 438L antioxidant.
  • Lubricant formulated in this matter having a TBN of 10.8 was subjected to the P-VW 3344 seal test and was found to yield passing results.
  • a lubricant is formulated as in Example IV with the exception that the AG dispersant is formed from a polyisobutenyl succinic anhydride in which the polyisobutenyl substituent is derived from the polyisobutene referred to in Example III.
  • Engine oil with a TBN of 9.1 formed in this manner gave passing results in the Peugeot TU3 test.
  • a finished crankcase lubricant is formulated to contain:
  • Example VI is repeated with the following changes:
  • the finished lubricant contains 1.31% of the mixed primary and secondary alkyl zinc dialkyl dithiophosphate of Example I in lieu of the zinc di-(secondary alkyl) dithiophosphate.
  • the detergent system in this finished lubricant is 2.60% of HiTEC® 611 additive and 0.64% of low-base calcium alkylbenzene sulfonate (HiTEC® 614 additive).
  • the antioxidant system in this finished lubricant is 0.80% of the methylene-bridged phenolic antioxidant of Example II and 0.25% of the bis (alkylphenyl) amine antioxidant of Example I.
  • the finished lubricant contains 0.004% of the methyl silicone foam inhibitor of Example 1 and 0.29% of additional separately added process oil diluent.
  • Lubricant formulated as in this example passed the P-VW 3344 seal test.
  • a lubricant is formed as in Example VII but substituting 7.0% of the AG dispersant of Example 3 for the AG dispersant of Example VII.
  • lubricant formulated in this manner was found to give passing results in the P-VW 3344 seal test.
  • oil-soluble means that the material can be dissolved in or be stably dispersed in the base oil used to at least the minimum concentration required for use as described herein.
  • the material has a solubility or dispersibility in the base oil well in excess of such minimum concentration.
  • oil-soluble does not signify that the material must dissolve or be dispersible in all proportions in the base oil.
  • additive components are supplied in the form of solutions of the active ingredient(s) in an inert diluent or solvent, such as a diluent oil.
  • a diluent oil such as a diluent oil
  • ashless dispersants and metal detergents are usually provided in the form of such solutions.
  • concentrations of each additive component are expressed on an "as received" basis -- i.e., the amount of solvent or diluent that may be associated with such component as received is included.
  • Total base numbers referred to herein are typically determined in accordance with ASTM test procedure D2896.

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Claims (18)

  1. Schmiermittelzusammensetzung umfassend einen größeren steil Öl mit Schmiermittelviskosität, umfassend:
    a) 0,03 bis 0,15 Gew.-% Stickstoff als öllösliches Produkt, das durch Umsetzung von Aminoguanidin und/oder einem basischen Salz davon mit einem acyclischen Hydrocarbylbernsteinsäureacylierungsmittel in einem Molverhältnis im Bereich von 0,4 bis 1,3 Mol Aminoguanidin und/oder einem basischen Salz hiervon pro Mol des Acylierungsmittels gebildet wurde;
    b) 0,08 bis 0,14 Gew.-% Zink als öllösliches Zinkdihydrocarbyldithiophosphat, wobei mindestens 35 Mol-% der anwesenden Hydrocarbylgruppen als sekundäre Hydrocarbylgruppen vorliegen; und
    c) 0,15 bis 0,40 Gew.-% Calcium als basisches Calciumdetergens-Additiv als Ergänzung, wobei mindestens 60 Mol-% des Calciums aus überbasischem Calciumdetergens mit einem TBN von mindestens 200 mg KOH/g stammen.
  2. Schmiermittelzusammensetzung nach Anspruch 1, das weiterhin bis zu 0,1 Gew.-% Magnesium als überbasisches Magnesiumdetergens-Additiv als Ergänzung umfaßt, und ein TBN von mindestens 300 mg KOH/g aufweist.
  3. Schmiermittelzusammensetzung nach Anspruch 1 oder Anspruch 2, wobei das TBN der Zusammensetzung im Bereich von 6 bis 15 mg KOH/g liegt.
  4. Schmiermittelzusammensetzung nach einem der vorstehenden Ansprüche, das weiterhin mindestens ein öllösliches Antioxidans und mindestens ein Antischäumungsmittel umfaßt.
  5. Schmiermittelzusammensetzung nach einem der vorstehenden Ansprüche, das weiterhin mindestens einen Viskositätsindexverbesserer umfaßt.
  6. Schmiermittelzusammensetzung nach einem der vorstehenden Ansprüche, bei dem das Zinkdihydrocarbyldithiophosphat ein Gemisch aus Zinkdialkyldithiophosphaten ist, wobei primäre und sekundäre Alkylgruppen vorliegen und mindestens 35 Mol-% der Alkylgruppen sekundäre Alkylgruppen sind.
  7. Schmiermittelzusammensetzung nach einem der vorstehenden Ansprüche, wobei das basische Calciumdetergens-Additiv als Ergänzung eine überbasische Calciumsulfonatdetergenszusammensetzung umfaßt, die einen TBN von mindestens 280 mg KOH/g aufweist.
  8. Schmiermittelzusammensetzung nach einem der vorstehenden Ansprüche, wobei das basische Calciumdetergens-Additiv als Ergänzung ein Gemisch aus i) und ii), oder i) und iii), oder i), ii) und iii) umfaßt, wobei:
    i) eine überbasische Calciumsulfonatdetergenszusammensetzung mit einem TBN von mindestens 280 mg KOH/g ist und in einer solchen Mengen vorliegt, daß mindestens 40 Gew.-% des Calciums hieraus stammen;
    ii) ein überbasische geschwefelte Calciumphenatdetergenszusammensetzung mit einem TBN von mindestens 100 mg KOH/g ist und, falls vorhanden, in einer solchen Menge vorliegt, daß bis zu 50 Gew.-% des Calciums hiervon stammen; und
    iii) ein niedrig-basisches Calciumsulfonatdetergens mit einem TBN von bis zu 40 mg KOH/g ist und, falls vorhanden, in einer Menge vorliegt, daß bis zu 25 Gew.-% des Calciums hiervon stammen.
  9. Schmiermittelzusammensetzung nach einem der vorstehenden Ansprüche, wobei das öllösliche Produkt durch Umsetzung von Aminoguanidin und/oder einem basischen Salz hiervon mit einem Alkenylbernsteinsäureacylierungsmittel in einem Molverhältnis im Bereich von 0,8 bis 1,2 Mol Aminoguanidin und/oder einem basischen Salz hiervon pro Mol des Acylierungsmittels gebildet wird, und die Alkenylgruppe des Acylierungsmittels aus einem Polyolefin stammt, das ein GPC-Molekulargewichtszahlenmittel im Bereich von 900 bis 2500 hat.
  10. Additiv-Konzentrat umfassend:
    a) 0,3 bis 0,8 Gew.-% Stickstoff als öllösliches Produkt, das durch Umsetzung von Aminoguanidin und/oder einem basischen Salz hiervon mit einem acyclischen Hydrocarbylbernsteinsäureacylierungsmittel in einem Molverhältnis im Bereich von 0,4 bis 1,3 Mol Aminoguanidin und/oder einem basischen Salz hiervon pro Mol des Acylierungsmittels erhalten wurde;
    b) 0,5 bis 1,2 Gew.-% Zink als öllösliches Zinkdihydrocarbyldithiophosphat, wobei mindestens 35 Mol-% der Hydrocarbylgruppen als sekundäre Hydrocarbylgruppen vorliegen; und
    c) 1,0 bis 4,0 Gew.-% Calcium als basisches Calciumdetergens-Additiv als Ergänzung, wobei mindestens 60 Mol-% des Calciums aus überbasischem Calcium-Detergens mit einem TBN von mindestens 200 mg KOH/g stammen.
  11. Additiv-Konzentrat nach Anspruch 10, weiterhin umfassend bis zu 0,8 Gew.-% Magnesium als überbasisches Magnesiumdetergens-Additiv als Ergänzung, das einen TBN von mindestens 300 mg KOH/g aufweist, und gegebenenfalls 0,5 bis 20 Gew.-% mindestens eines öllöslichen Antioxidans, und gegebenenfalls 0,001 bis 0,05 Gew.-% mindestens eines Antischäumungsmittels.
  12. Additiv-Konzentrat nach Anspruch 10 oder Anspruch 11, wobei der TBN des Konzentrats im Bereich von 50 bis 120 mg KOH/g liegt.
  13. Additiv-Konzentrat nach einem der Ansprüche 10 bis 12, wobei das Zinkdihydrocarbyldithiophosphat als ein Gemisch aus Zinkdialkyldithiophosphaten vorliegt, wobei primäre und sekundäre Alkylgruppen anwesend sind, und mindestens 35 Mol-% der Alkylgruppen sekundäre Alkylgruppen sind.
  14. Additiv-Konzentrat nach einem der Ansprüche 10 bis 13, wobei das basische Calciumdetergens-Additiv als Ergänzung eine überbasische Calciumsulfonatdetergens-Zusammensetzung mit einem TBN von mindestens 280 mg KOH/g umfaßt.
  15. Additiv-Konzentrat nach einem der Ansprüche 10 bis 14, wobei das basische Calciumdetergens-Additiv als Ergänzung ein Gemisch aus i) und ii), oder i) und iii), oder i), ii) und iii) umfaßt, wobei:
    i) eine überbasische Calciumsulfonatdetergens-Zusammensetzung mit einem TBN von mindestens 280 mg KOH/g hiervon ist und in einer solchen Menge anwesend ist, daß mindestens 40 Gew.-% Calcium hiervon stammen;
    ii) eine überbasische geschwefelte Calciumphenatdetergens-Zusammensetzung mit einem TBN von mindestens 100 mg KOH/g ist, und, wenn anwesend, in einer solchen Menge vorhanden sind, daß bis zu 50 Gew.-% des Calciums hiervon stammen; und
    iii) ein niedrig-basisches Calciumsulfonatdetergens mit einem TBN von bis zu 40 mg KOH/g ist, und, wenn anwesend, in einer solchen Menge vorhanden ist, daß bis zu 25 Gew.-% des Calciums hiervon stammen.
  16. Additiv-Konzentrat nach einem der Ansprüche 10 bis 15, wobei das öllösliche Produkt durch Umsetzung von Aminoguanidin und/oder einem basischen Salz hiervon mit einem Alkenylbernsteinsäureacylierungsmittel in einem Molverhältnis im Bereich von 0,8 bis 1,2 Mol Aminoguanidin und/oder einem basischen Salz hiervon pro Mol Acylierungsmittel gebildet wurde und die Alkenylgruppe des Acylierungsmittels aus einem Polyolefin mit einem GPC-Molekulargewichtszahlenmittel im Bereich von 900 bis 2500 abgeleitet sind.
  17. Verwendung einer Schmiermittelzubereitung nach einem der Ansprüche 1 bis 9 oder eines Additiv-Konzentrats nach einem der Ansprüche 10 bis 16 zur Formulierung einer Motorölzusammensetzung, die mindestens den Sequence-VE-Motortest, den P-VW 5106-Test, den L-38-Motortest, den P-VW 1431-Motortest, den P-VW 3344-Dichtungstest und den P-VW 1302-Motortest besteht.
  18. Verwendung einer Schmiermittelzubereitung nach einem der Ansprüche 1 bis 9 oder eines Additiv-Konzentrats nach einem der Ansprüche 10 bis 16 zur Formulierung einer Motorölzubereitung, die mindestens den Peugeot TU3-Test, den P-VW 3344-Dichtungstest, den M-B NBR-34-Dichtungstest, den M-B AK-6-Dichtungstest, den MAN NBR-28-Dichtungstest und den MAN AK-6-Dichtungstest besteht.
EP94305974A 1993-08-13 1994-08-12 Motorölzusammensetzungen, Zusatzkonzentrat zur Herstellung solcher Öle und ihre Verwendung Expired - Lifetime EP0638632B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9316985A GB2280907B (en) 1993-08-13 1993-08-13 Motor oil compositions,additive concentrates for producing such motor oils,and the use thereof
GB9316985 1993-08-13

Publications (3)

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EP0638632A2 EP0638632A2 (de) 1995-02-15
EP0638632A3 EP0638632A3 (de) 1995-07-05
EP0638632B1 true EP0638632B1 (de) 2000-03-01

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EP (1) EP0638632B1 (de)
JP (1) JPH07150185A (de)
AU (1) AU670883B2 (de)
CA (1) CA2130035A1 (de)
DE (1) DE69423153D1 (de)
GB (1) GB2280907B (de)

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US10214703B2 (en) 2015-07-16 2019-02-26 Afton Chemical Corporation Lubricants with zinc dialkyl dithiophosphate and their use in boosted internal combustion engines
US10280383B2 (en) 2015-07-16 2019-05-07 Afton Chemical Corporation Lubricants with molybdenum and their use for improving low speed pre-ignition
US10550349B2 (en) 2015-07-16 2020-02-04 Afton Chemical Corporation Lubricants with titanium and/or tungsten and their use for improving low speed pre-ignition
US11155764B2 (en) 2016-05-05 2021-10-26 Afton Chemical Corporation Lubricants for use in boosted engines

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WO1997010318A1 (en) * 1995-09-14 1997-03-20 Exxon Chemical Patents Inc. Crankcase lubricating compositions
US5747433A (en) * 1996-07-15 1998-05-05 The Lubrizol Corporation Oil concentrates of polymers with improved viscosity
US6841521B2 (en) * 2003-03-07 2005-01-11 Chevron Oronite Company Llc Methods and compositions for reducing wear in heavy-duty diesel engines
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US8623105B2 (en) 2008-05-13 2014-01-07 Afton Chemical Corporation Fuel additives to maintain optimum injector performance
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US10421922B2 (en) * 2015-07-16 2019-09-24 Afton Chemical Corporation Lubricants with magnesium and their use for improving low speed pre-ignition
US10336959B2 (en) 2015-07-16 2019-07-02 Afton Chemical Corporation Lubricants with calcium-containing detergent and their use for improving low speed pre-ignition
US10377963B2 (en) 2016-02-25 2019-08-13 Afton Chemical Corporation Lubricants for use in boosted engines
US10370615B2 (en) 2017-01-18 2019-08-06 Afton Chemical Corporation Lubricants with calcium-containing detergents and their use for improving low-speed pre-ignition
US10443011B2 (en) 2017-01-18 2019-10-15 Afton Chemical Corporation Lubricants with overbased calcium and overbased magnesium detergents and method for improving low-speed pre-ignition
US10443558B2 (en) 2017-01-18 2019-10-15 Afton Chemical Corporation Lubricants with calcium and magnesium-containing detergents and their use for improving low-speed pre-ignition and for corrosion resistance

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US10214703B2 (en) 2015-07-16 2019-02-26 Afton Chemical Corporation Lubricants with zinc dialkyl dithiophosphate and their use in boosted internal combustion engines
US10280383B2 (en) 2015-07-16 2019-05-07 Afton Chemical Corporation Lubricants with molybdenum and their use for improving low speed pre-ignition
US10550349B2 (en) 2015-07-16 2020-02-04 Afton Chemical Corporation Lubricants with titanium and/or tungsten and their use for improving low speed pre-ignition
US11155764B2 (en) 2016-05-05 2021-10-26 Afton Chemical Corporation Lubricants for use in boosted engines

Also Published As

Publication number Publication date
EP0638632A3 (de) 1995-07-05
GB9316985D0 (en) 1993-09-29
EP0638632A2 (de) 1995-02-15
CA2130035A1 (en) 1995-02-14
GB2280907B (en) 1997-04-30
GB2280907A (en) 1995-02-15
AU7025094A (en) 1995-02-23
DE69423153D1 (de) 2000-04-06
JPH07150185A (ja) 1995-06-13
AU670883B2 (en) 1996-08-01

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