EP0616635B1 - Brennstoffzusammensetzung für zweitaktmotoren - Google Patents

Brennstoffzusammensetzung für zweitaktmotoren Download PDF

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Publication number
EP0616635B1
EP0616635B1 EP93921434A EP93921434A EP0616635B1 EP 0616635 B1 EP0616635 B1 EP 0616635B1 EP 93921434 A EP93921434 A EP 93921434A EP 93921434 A EP93921434 A EP 93921434A EP 0616635 B1 EP0616635 B1 EP 0616635B1
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EP
European Patent Office
Prior art keywords
molybdenum
sulfur
carboxylic acid
basic nitrogen
fuel composition
Prior art date
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Expired - Lifetime
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EP93921434A
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English (en)
French (fr)
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EP0616635A1 (de
EP0616635A4 (de
Inventor
Glenn E. Callis
Edward T. Sabourin
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Chevron Phillips Chemical Co LP
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Chevron Chemical Co LLC
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    • C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/09—Complexes with metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • 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
    • C10N2040/26—Two-strokes or two-cycle engines
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02B—INTERNAL-COMBUSTION PISTON ENGINES; COMBUSTION ENGINES IN GENERAL
    • F02B75/00—Other engines
    • F02B75/02—Engines characterised by their cycles, e.g. six-stroke
    • F02B2075/022—Engines characterised by their cycles, e.g. six-stroke having less than six strokes per cycle
    • F02B2075/025—Engines characterised by their cycles, e.g. six-stroke having less than six strokes per cycle two

Definitions

  • the present invention relates to a fuel composition for two-cycle internal combustion engines which comprises a major amount of fuel boiling in the gasoline range and a minor amount of a lubricant composition comprising a lubricating oil and an additive formulation containing a molybdenum/sulfur complex of a basic nitrogen compound.
  • spark-ignited two-cycle (two-stroke) internal combustion engines including rotary engines such as those of the Wankel type has steadily increased. They are presently found in power lawn mowers and other power-operated garden equipment, power chain saws, pumps, electrical generators, marine outboard engines, snowmobiles, motorcycles, and the like.
  • U.S. Patent No. 4,708,809 to Davis discloses a lubricant composition for two-cycle engines comprising a major amount of an oil of lubricating viscosity and a minor amount of at least one alkyl phenol having at least one hydrocarbon-based group of at least 10 aliphatic carbon atoms.
  • such lubricant composition will also contain a detergent-dispersant additive selected from (i) a neutral or basic metal salt of an organic sulfur acid, phenol or carboxylic acid, (ii) a hydrocarbyl-substituted amine, (iii) an acylated, nitrogen-containing compound having a substituent of at least 10 aliphatic carbon atoms, (iv) a nitrogen-containing condensate of a phenol, aldehyde and amino compound, and (v) an ester of a substituted polycarboxylic acid.
  • a detergent-dispersant additive selected from (i) a neutral or basic metal salt of an organic sulfur acid, phenol or carboxylic acid, (ii) a hydrocarbyl-substituted amine, (iii) an acylated, nitrogen-containing compound having a substituent of at least 10 aliphatic carbon atoms, (iv) a nitrogen-containing condensate of a phenol, aldehyde
  • U.S. Patent No. 4,724,091 to Davis discloses a lubricant composition for two-cycle engines comprising a major amount of an oil of lubricating viscosity and a minor amount of a mixture of at least one alkyl phenol and at least one amino phenol, each phenol having at least one hydrocarbon-based group of at least about 10 aliphatic carbon atoms.
  • this composition will additionally contain a detergent-dispersant additive.
  • U.S. Patent No. 4,740,321 to Davis et al. discloses a lubricant composition for two-cycle engines comprising a major amount of an oil of lubricating viscosity and a minor amount of at least one sulfurized alkyl phenol or metal salt thereof having at least one hydrocarbon-based group of at least 10 aliphatic carbon atoms.
  • This lubricant composition will also preferably contain a detergent-dispersant additive.
  • U.S. Patent No. 4,705,643 to Nemo discloses a lubricating oil composition for two-cycle engines comprising a lubricating oil and an ashless detergent additive which is the hydrolyzed reaction product of an aliphatic branched chain carboxylic acid of 16 to 20 carbon atoms and a polyamine of at least 3 amine groups.
  • the ashless detergent additive is the hydrolyzed reaction product of isostearic acid and tetraethylenepentamine.
  • U.S. Patent No. 4,994,196 to Kagaya et al. discloses a two-cycle engine oil composition comprising a base oil and a calcium phenate detergent additive, wherein the base oil is a mixture of (a) a copolymer of an alpha-olefin with an ester of a dicarboxylic acid and (b) an ester of pentaerythritol and a fatty acid.
  • U.S. Patent No. 3,888,776 to Silverstein discloses a two-cycle engine lubricant which comprises a major amount of a polypropylene glycol and minor amounts of a sulfurized oxymolybdenum organophosphorodithioate, a finely divided molybdenum disulfide and a halogenated hydrocarbon detergent, such as 1,1,1-trichloroethylene, orthodichlorobenzene, perchlorinated biphenyl, and the like.
  • Molybdenum/sulfur complexes of basic nitrogen compounds have previously been described in the art as useful antioxidant additives for lubricant compositions finding application, for example, as crosshead diesel engine lubricants, automobile and railroad crankcase lubricants, lubricants for heavy machinery, greases for bearings, and the like.
  • U.S. Patent No. 4,263,152 to King et al. discloses an antioxidant additive for lubricating oils which is prepared by combining an acidic molybdenum compound, a polar promoter, a basic nitrogen-containing compound and a sulfur source to form a molybdenum and sulfur-containing complex. Similar molybdenum-containing antioxidant additives are disclosed in U.S. Patent Nos. 4,285,822; 4,283,295; 4,272,387; 4,265,773; 4,261,843; 4,259,195; and 4,259,194.
  • the present invention is directed to minimizing the problems of varnish build-up and ring sticking in two-cycle engines through the provision of effective additives for fuel-lubricating oil combinations which eliminate or reduce two-cycle engine varnish deposits and piston ring seal failure.
  • the present invention provides a fuel composition for two-cycle engines comprising a major amount of fuel boiling in the gasoline range and a minor amount of a lubricant composition comprising:
  • the fuel composition of the present invention will comprise a major amount of fuel boiling in the gasoline range and a minor amount of a lubricant composition comprising a base oil of lubricating viscosity and an additive formulation containing (1) a sulfurized molybdenum-containing composition, (2) a carboxylic acid amide, and (3) a succinimide.
  • the sulfurized molybdenum-containing composition employed in the present invention may be generally characterized as a molybdenum/sulfur complex of a basic nitrogen compound.
  • molybdenum/sulfur complexes are known in the art and are described, for example, in U.S. Patent No. 4,263,152 to King et al.
  • molybdenum compositions employed in this invention are not known with certainty; however, they are believed to be compounds in which molybdenum, whose valences are satisfied with atoms of oxygen or sulfur, is either complexed by, or the salt of, one or more nitrogen atoms of the basic nitrogen containing compound used in the preparation of these compositions.
  • the molybdenum compounds used to prepare the molybdenum/sulfur complexes employed in this invention are acidic molybdenum compounds.
  • acidic is meant that the molybdenum compounds will react with a basic nitrogen compound as measured by ASTM test D-664 or D-2896 titration procedure.
  • molybdenum compounds are hexavalent and are represented by the following compositions: molybdic acid, ammonium molybdate, sodium molybdate, potassium molybdate and other alkaline metal molybdates and other molybdenum salts such as hydrogen salts, e.g., hydrogen sodium molybdate, MoOCl 4 , MoO 2 Br 2 , Mo 2 O 3 Cl 6 , molybdenum trioxide or similar acidic molybdenum compounds.
  • Preferred acidic molybdenum compounds are molybdic acid, ammonium molybdate, and alkali metal molybdates. Particularly preferred are molybdic acid and ammonium molybdate.
  • the basic nitrogen compound used to prepare the molybdenum/sulfur complexes must have a basic nitrogen content as measured by ASTM D-664 or D-2896. It is preferably oil-soluble. Typical of such compositions are succinimides, carboxylic acid amides, hydrocarbyl monoamines, hydrocarbon polyamines, Mannich bases, phosphoramides, thiophosphoramides, phosphonamides, and mixtures thereof. These basic nitrogen-containing compounds are described below (keeping in mind the reservation that each must have at least one basic nitrogen). Any of the nitrogen-containing compositions may be after-treated with, e.g., boron, using procedures well known in the art so long as the compositions continue to contain basic nitrogen. These after-treatments are particularly applicable to succinimides and Mannich base compositions.
  • succinimide The mono and polysuccinimides that can be used to prepare the molybdenum/sulfur complexes described herein are disclosed in numerous references and are well known in the art. Certain fundamental types of succinimides and the related materials encompassed by the term of art "succinimide" are taught in U.S. Patent Nos. 3,219,666; 3,172,892; and 3,272,746. The term “succinimide” is understood in the art to include many of the amide, imide, and amidine species which may also be formed. The predominant product however is a succinimide and this term has been generally accepted as meaning the product of a reaction of an alkenyl substituted succinic acid or anhydride with a nitrogen-containing compound.
  • Preferred succinimides because of their commercial availability, are those succinimides prepared from a hydrocarbyl succinic anhydride, wherein the hydrocarbyl group contains from about 24 to about 350 carbon atoms, and an ethylene amine, said ethylene amines being especially characterized by ethylene diamine, diethylene triamine, triethylene tetramine, and tetraethylene pentamine.
  • Particularly preferred are those succinimides prepared from polyisobutenyl succinic anhydride of 70 to 128 carbon atoms and tetraethylene pentamine or triethylene tetramine or mixtures thereof.
  • succinimide also included within the term “succinimide” are the cooligomers of a hydrocarbyl succinic acid or anhydride and a poly secondary amine containing at least one tertiary amino nitrogen in addition to two or more secondary amino groups. Ordinarily this composition has between 1,500 and 50,000 average molecular weight.
  • a typical compound would be that prepared by reacting polyisobutenyl succinic anhydride and ethylene dipiperazine.
  • Carboxylic acid amide compositions are also suitable starting materials for preparing the molybdenum/sulfur complexes employed in this invention. Typical of such compounds are those disclosed in U.S. Patent No. 3,405,064. These compositions are ordinarily prepared by reacting a carboxylic acid or anhydride or ester thereof, having at least 12 to about 350 aliphatic carbon atoms in the principal aliphatic chain and, if desired, having sufficient pendant aliphatic groups to render the molecule oil soluble with an amine or a hydrocarbyl polyamine, such as an ethylene amine, to give a mono or polycarboxylic acid amide.
  • hydrocarbyl monoamines and hydrocarbyl polyamines preferably of the type disclosed in U.S. Patent No. 3,574,576.
  • the hydrocarbyl group which is preferably alkyl, or olefinic having one or two sites of unsaturation, usually contains from 9 to 350, preferably from 20 to 200 carbon atoms.
  • hydrocarbyl polyamines are those which are derived, e.g., by reacting polyisobutenyl chloride and a polyalkylene polyamine, such as an ethylene amine, e.g., ethylene diamine, diethylene triamine, tetraethylene pentamine, 2-aminoethylpiperazine, 1,3-propylene diamine, 1,2-propylenediamine, and the like.
  • a polyalkylene polyamine such as an ethylene amine, e.g., ethylene diamine, diethylene triamine, tetraethylene pentamine, 2-aminoethylpiperazine, 1,3-propylene diamine, 1,2-propylenediamine, and the like.
  • Mannich base compositions Another class of compounds useful for supplying basic nitrogen are the Mannich base compositions. These compositions are prepared from a phenol or C 9-200 alkylphenol, an aldehyde, such as formaldehyde or formaldehyde precursor such as paraformaldehyde, and an amine compound.
  • the amine may be a mono or polyamine and typical compositions are prepared from an alkylamine, such as methylamine or an ethylene amine, such as, diethylene triamine, or tetraethylene pentamine, and the like.
  • the phenolic material may be sulfurized and preferably is dodecylphenol or a C 80-100 alkylphenol.
  • Typical Mannich bases which can be used in this invention are disclosed in U.S. Patent No.
  • Mannich bases prepared by reacting an alkylphenol having at least 50 carbon atoms, preferably 50 to 200 carbon atoms with formaldehyde and an alkylene polyamine HN(ANH) n H where A is a saturated divalent alkyl hydrocarbon of 2 to 6 carbon atoms and n is 1-10 and where the condensation product of said alkylene polyamine may be further reacted with urea or thiourea.
  • A is a saturated divalent alkyl hydrocarbon of 2 to 6 carbon atoms and n is 1-10 and where the condensation product of said alkylene polyamine may be further reacted with urea or thiourea.
  • the utility of these Mannich bases as starting materials for preparing lubricating oil additives can often be significantly improved by treating the Mannich base using conventional techniques to introduce boron into the composition.
  • compositions useful for preparing the molybdenum/sulfur complexes employed in this invention are the phosphoramides and phosphonamides such as those disclosed in U.S. Patent Nos. 3,909,430 and 3,968,157. These compositions may be prepared by forming a phosphorus compound having at least one P-N bond. They can be prepared, for example, by reacting phosphorus oxychloride with a hydrocarbyl diol in the presence of a monoamine or by reacting phosphorus oxychloride with a difunctional secondary amine and a mono-functional amine.
  • Thiophosphoramides can be prepared by reacting an unsaturated hydrocarbon compound containing from 2 to 450 or more carbon atoms, such as polyethylene, polyisobutylene, polypropylene, ethylene, 1-hexene, 1,3-hexadiene, isobutylene, 4-methyl-1-pentene, and the like, with phosphorus pentasulfide and a nitrogen-containing compound as defined above, particularly an alkylamine, alkyldiamine, alkylpolyamine, or an alkyleneamine, such as ethylene diamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, and the like.
  • an unsaturated hydrocarbon compound containing from 2 to 450 or more carbon atoms such as polyethylene, polyisobutylene, polypropylene, ethylene, 1-hexene, 1,3-hexadiene, isobutylene, 4-methyl-1-pentene, and the like
  • VI improvers dispersant viscosity index improvers
  • hydrocarbon polymer especially a polymer derived from ethylene and/or propylene, optionally containing additional units derived from one or more co-monomers such as alicyclic or aliphatic olefins or diolefins.
  • the functionalization may be carried out by a variety of processes which introduce a reactive site or sites which usually has at least one oxygen atom on the polymer.
  • the polymer is then contacted with a nitrogen-containing source to introduce nitrogen-containing functional groups on the polymer backbone.
  • Commonly used nitrogen sources include any basic nitrogen compound especially those nitrogen-containing compounds and compositions described herein.
  • Preferred nitrogen sources are alkylene amines, such as ethylene amines, alkyl amines, and Mannich bases.
  • Preferred basic nitrogen compounds for use in this invention are succinimides, carboxylic acid amides, and Mannich bases.
  • Representative sulfur sources for preparing the molybdenum complexes used in this invention are sulfur, hydrogen sulfide, sulfur monochloride, sulfur dichloride, phosphorus pentasulfide, R 2 S x where R is hydrocarbyl, preferably C 1-40 alkyl, and x is at least 2, inorganic sulfides and polysulfides such as (NH 4 ) 2 S x , where x is at least 1, thioacetamide, thiourea, and mercaptans of the formula RSH where R is as defined above.
  • sulfurizing agents are traditional sulfur-containing antioxidants such as wax sulfides and polysulfides, sulfurized olefins, sulfurized carboxylic and esters and sulfurized ester-olefins, and sulfurized alkylphenols and the metal salts thereof.
  • the sulfurized fatty acid esters are prepared by reacting sulfur, sulfur monochloride, and/or sulfur dichloride with an unsaturated fatty ester under elevated temperatures.
  • Typical esters include C 1 -C 20 alkyl esters of C 8 -C 24 unsaturated fatty acids, such as palmitoleic, oleic, ricinoleic, petroselinic, vaccenic, linoleic, linolenic, oleostearic, licanic, paranaric, tariric, gadoleic, arachidonic, cetoleic, etc.
  • mixed unsaturated fatty acid esters such as are obtained from animal fats and vegetable oils, such as tall oil, linseed oil, olive oil, caster oil, peanut oil, rape oil, fish oil, sperm oil, and so forth.
  • Exemplary fatty esters include lauryl tallate, methyl oleate, ethyl oleate, lauryl oleate, cetyl oleate, cetyl linoleate, lauryl ricinoleate, oleyl linoleate, oleyl stearate, and alkyl glycerides.
  • Cross-sulfurized ester olefins such as a sulfurized mixture of C 10 -C 25 olefins with fatty acid esters of C 10 -C 25 fatty acids and C 1 -C 25 alkyl or alkenyl alcohols, wherein the fatty acid and/or the alcohol is unsaturated may also be used.
  • Sulfurized olefins are prepared by the reaction of the C 3 -C 6 olefin or a low-molecular-weight polyolefin derived therefrom with a sulfur-containing compound such as sulfur, sulfur monochloride, and/or sulfur dichloride.
  • aromatic and alkyl sulfides such as dibenzyl sulfide, dixylyl sulfide, dicetyl sulfide, diparaffin wax sulfide and polysulfide, cracked wax-olefin sulfides and so forth.
  • They can be prepared by treating the starting material, e.g., olefinically unsaturated compounds, with sulfur, sulfur monochloride, and sulfur dichloride.
  • the paraffin wax thiomers described in U.S. Patent No. 2,346,156.
  • Sulfurized alkyl phenols and the metal salts thereof include compositions such as sulfurized dodecylphenol and the calcium salts thereof.
  • the alkyl group ordinarily contains from 9-300 carbon atoms.
  • the metal salt may be preferably, a Group I or Group II salt, especially sodium, calcium, magnesium, or barium.
  • Preferred sulfur sources are sulfur, hydrogen sulfide, phosphorus pentasulfide, R 2 S x where R is hydrocarbyl, preferably C 1 -C 10 alkyl, and x is at least 3, mercaptans wherein R is C 1 -C 10 alkyl, inorganic sulfides and polysulfides, thioacetamide, and thiourea.
  • Most preferred sulfur sources are sulfur, hydrogen sulfide, phosphorus pentasulfide, and inorganic sulfides and polysulfides.
  • the polar promoter used in the preparation of the molybdenum complexes employed in this invention is one which facilitates the interaction between the acidic molybdenum compound and the basic nitrogen compound.
  • a wide variety of such promoters are well known to those skilled in the art.
  • Typical promoters are 1,3-propanediol, 1,4-butane-diol, diethylene glycol, butyl cellosolve, propylene glycol, 1,4-butyleneglycol, methyl carbitol, ethanolamine, diethanolamine, N-methyl-diethanol-amine, dimethyl formamide, N-methyl acetamide, dimethyl acetamide, methanol, ethylene glycol, dimethyl sulfoxide, hexamethyl phosphoramide, tetrahydrofuran and water.
  • Preferred are water and ethylene glycol. Particularly preferred is water.
  • the polar promoter is separately added to the reaction mixture, it may also be present, particularly in the case of water, as a component of non-anhydrous starting materials or as waters of hydration in the acidic molybdenum compound, such as (NH 4 ) 6 Mo 7 O 24 .4 H 2 O. Water may also be added as ammonium hydroxide.
  • a method for preparing the molybdenum/sulfur complexes used in this invention is to prepare a solution of the acidic molybdenum precursor and a polar promoter with a basic nitrogen-containing compound with or without diluent.
  • the diluent is used, if necessary, to provide a suitable viscosity for easy stirring.
  • Typical diluents are lubricating oil and liquid compounds containing only carbon and hydrogen.
  • ammonium hydroxide may also be added to the reaction mixture to provide a solution of ammonium molybdate. This reaction is carried out at a temperature from the melting point of the mixture to reflux temperature. It is ordinarily carried out at atmospheric pressure although higher or lower pressures may be used if desired.
  • This reaction mixture is treated with a sulfur source as defined above at a suitable pressure and temperature for the sulfur source to react with the acidic molybdenum and basic nitrogen compounds. In some cases, removal of water from the reaction mixture may be desirable prior to completion of reaction with the sulfur source.
  • the ratio of molybdenum compound to basic nitrogen compound is not critical; however, as the amount of molybdenum with respect to basic nitrogen increases, the filtration of the product becomes more difficult. Since the molybdenum component probably oligomerizes, it is advantageous to add as much molybdenum as can easily be maintained in the composition.
  • the reaction mixture will have charged to it from 0.01 to 2.00 atoms of molybdenum per basic nitrogen atom.
  • the sulfur source is usually charged to the reaction mixture in such a ratio to provide 1.5 to 4.0 atoms of sulfur per atom of molybdenum.
  • the polar promoter which is preferably water, is ordinarily present in the ratio of 0.1 to 50 moles of promoter per mole of molybdenum. Preferably from 0.5 to 25 and most preferably 1.0 to 15 moles of the promoter is present per mole of molybdenum.
  • the additive formulation employed in the present invention contains (1) a sulfurized molybdenum-containing composition, (2) a carboxylic acid amide, and (3) a succinimide.
  • the carboxylic amide component of the presently employed additive formulation may be any of the carboxylic acid amide compounds described herein as useful in the preparation of the molybdenum/sulfur complex.
  • Preferred carboxylic acid amide components include those amides derived from a carboxylic acid of the formula R 2 COOH, wherein R 2 is C 12 -C 20 alkyl, and an ethylene amine, such as triethylene tetramine or tetraethylene pentamine.
  • the succinimide component of the presently employed additive formulation may be any of the succinimide compounds described herein as useful in the preparation of the molybdenum/sulfur complex.
  • Preferred succinimide components include those derived from polyisobutenyl succinic anhydride, wherein the polyisobutenyl group contains from about 50 to 250 carbon atoms, and an ethylene amine, such as triethylene tetramine or tetraethylene pentamine.
  • the additive formulation employed in the present invention may additionally contain a flocculant inhibitor and/or a lubricity agent, such as a polyisobutene. If necessary, a diluent oil may also be included.
  • additives such as viscosity index improvers, antioxidants, dispersants, coupling agents, pour point depressants, extreme pressure agents, color stabilizers, rust inhibitors, anticorrosion agents, and the like, may also be present in the additive formulation.
  • the lubricant composition employed in the present invention comprises a major amount of a base oil of lubricating viscosity and a minor amount of the additive formulation described above.
  • the base oil employed may be any of a wide variety of oils of lubricating viscosity.
  • the base oil can be a refined paraffin type base oil, a refined naphthenic base oil, or a synthetic hydrocarbon or non-hydrocarbon oil of lubricating viscosity.
  • the base oil can also be a mixture of mineral and synthetic oils.
  • the mineral lubricating oils are preferred, since they are presently in more general use in two-cycle engines.
  • the presently employed lubricant composition containing the additive formulation described herein can be conveniently prepared using conventional techniques by admixing the appropriate amount of each component of the additive formulation with a lubricating oil.
  • the amount of the molybdenum-containing additive will vary from about 0.05 to 15% by weight and preferably from about 0.2 to 10% by weight, based on the total lubricant composition, including base oil.
  • the carboxylic acid amide component will vary from about 0.05 to 20% by weight and preferably from about 0.2 to 15% by weight.
  • the succinimide component will vary from about 0.5 to 15% by weight and preferably from about 0.2 to 10% by weight.
  • the two-cycle engine fuel composition contemplated by the present invention comprises a major amount of fuel boiling in the gasoline range and minor amount of the lubricant composition disclosed herein.
  • the lubricant composition will generally be added directly to the fuel to form a mixture of lubricant and fuel which is then introduced into the two-cycle engine cylinder.
  • the resulting fuel composition will contain from about 15 to 250 parts fuel per 1 part lubricant, and more typically about 50 to 100 parts fuel per 1 part lubricant.
  • the lubricant may be directly injected into the combustion chamber along with the fuel or into the fuel just prior to the time the fuel enters the combustion chamber.
  • the fuel employed in the present fuel composition is a hydrocarbon distillate fuel boiling in the gasoline range.
  • other fuel additives may also be included such as antiknock agents, e.g., methylcyclopentadienyl manganese tricarbonyl, tetramethyl or tetraethyl lead, or other dispersants or detergents such as various substituted amines, etc.
  • lead scavengers such as aryl halides, e.g., dichlorobenzene or alkyl halides, e.g., ethylene dibromide.
  • antioxidants, metal deactivators, pour point depressants, corrosion inhibitors and demulsifiers may be present.
  • the molybdenum/sulfur complexes of Examples 1, 2 and 4 were formulated to provide lubricant compositions containing 10% of the carboxylic acid amide reaction product of isostearic acid and tetraethylene pentamine, 2% of a polyisobutenyl succinimide prepared from polyisobutenyl succinic anhydride wherein the polyisobutenyl group has a number average molecular weight of about 950 and tetraethylene pentamine, 2% of the molybdenum/sulfur complex of Examples 1, 2 and 4, respectively, 5% of a polyisobutene having a number average molecular weight of about 950 as a lubricity agent, 0.5% of a flocculant inhibitor, 1% of a diluent oil and about 79.5% of a base oil.
  • the base oil contains about 10% of a 150 bright stock, about 70% of a mixture of 350N and 650N neutral oils, and about 20% of a petroleum distillate
  • test engine used was an Outboard Marine Company Johnson Model No. J70ELEIE outboard engine, which is a 70 horsepower, water-cooled, three-cylinder, two-cycle engine.
  • test procedure involved a two-hour break-in period, wherein the engine was run at 3,000 rpm for 1 hour, then at 4,000 rpm for 1 hour, using a fuel:lubricant ratio of 50:1.
  • test was then conducted for 98 hours using a 50:1 fuel to lubricant ratio on a 55 minute wide-open throttle, 5 minute idle cycle.
  • the total test time, including break-in, was 100 hours.
  • the second-ring sticking values include a National Marine Manufacturers Association (NMMA) rating, a visual rating, and an adjusted rating, which is an average of the NMMA and visual ratings.
  • NMMA National Marine Manufacturers Association
  • the reference oil employed in this test was NMMA reference oil TCW II, used as an industry standard in two-cycle engine tests to measure engine cleanliness.
  • the TCW II reference oil is a standard mineral lubricating oil containing a commercial ashless dispersant for gasoline two-cycle engines.
  • the reference oil is available from Citgo Petroleum Corporation, Tulsa, Oklahoma.

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Claims (36)

  1. Treibstoffzusammensetzung für Zweitaktmotoren, umfassend eine größere Menge eines im Benzinbereich siedenden Treibstoffs und eine geringere Menge einer Schmiermittelzusammensetzung, umfassend:
    (A) eine größere Menge eines Basisöls mit Schmierviskosität, und
    (B) eine kleinere Menge einer Additiv-Formulierung, umfassend:
    (1) 0,05 bis 15 Gew.% einer sulfurierten molybdänhaltigen Zusammensetzung, hergestellt durch (i) Umsetzen einer sauren Molybdänverbindung und einer basischen Stickstoffverbindung, ausgewählt aus der Gruppe Succinimid, Carbonsäureamid, Kohlenwasserstoffmonoamin, Kohlenwasserstoffpolyamin, Mannich-Base, Phosphoramid, Thiophosphoramid, Phosphonamid oder einem Gemisch davon, in Gegenwart eines polaren Aktivators, so dass ein Molybdänkomplex entsteht, wobei 0,01 bis 2 Molybdänatome pro basischem Stickstoffatom zugegen sind, und der Aktivator im Verhältnis von 0,01 bis 50 Mol polarer Aktivator pro Mol Molybdän zugegen ist; und (ii) Umsetzen des Molybdänkomplexes mit einer schwefelhaltigen Verbindung in einer Menge, die ausreicht, dass etwa 1,5 bis 4,0 Schwefelatome pro Molybdänatom bereitgestellt werden, wodurch eine schwefel- und molybdänhaltige Zusammensetzung entsteht,
    (2) 0,05 bis 20 Gew.% eines Carbonsäureamides, und
    (3) 0,05 bis 15 Gew.% eines Succinimides.
  2. Treibstoffzusammensetzung nach Anspruch 1, wobei die Schwefelquelle für Komponente (1) ist: Schwefel, Schwefelwasserstoff, Phosphorpentasulfid, R2Sx, wobei R Kohlenwasserstoff ist, und x mindestens 2 ist, anorganische Sulfide oder anorganische Polysulfide, Thioacetamid, Thioharnstoff, Mercaptane der Formel RSH, wobei R Kohlenwasserstoff ist, oder ein schwefelhaltiges Antioxidans.
  3. Treibstoffzusammensetzung nach Anspruch 2, wobei die Schwefelquelle für Komponente (1) ist: Schwefel, Schwefelwasserstoff, Phosphorpentasulfid, R2Sx, wobei R C1-4-Kohlenwasserstoff ist, und x mindestens 3 ist, anorganische Sulfide oder anorganische Polysulfide, Thioacetamid, Thioharnstoff, oder RSH, wobei R C1-40-Alkyl ist, und die saure Molybdänverbindung Molybdänsäure, Ammoniummolybdat oder Alkalimetallmolybdat ist.
  4. Treibstoffzusammensetzung nach Anspruch 3, wobei die Schwefelquelle Schwefel, Schwefelwasserstoff, RSH, wobei R C1-10-Alkyl ist, Phosphorpentasulfid oder (NH4)2Sx, ist, wobei x' mindestens 1 ist, die saure Molybdänverbindung Molybdänsäure oder Ammoniummolybdat ist, und die Stickstoffverbindung ein Succinimid, Carbonsäureamid oder eine Mannich-Base ist.
  5. Treibstoffzusammensetzung nach Anspruch 4, wobei die basische Stickstoffverbindung ein C24-350 -Kohlenwasserstoff-Succinimid, ein Carbonsäureamid oder eine Mannich-Base ist, die aus einem C9-200-Alkylphenol, Formaldehyd und einem Amin hergestellt ist.
  6. Treibstoffzusammensetzung nach Anspruch 5, wobei die basische Stickstoff-Verbindung ein Polyisobutenyl-Succinimid ist, das hergestellt ist aus Polyisobutenyl-Bernsteinsäureanhydrid und Tetraethylenpentamin oder Triethylentetramin.
  7. Treibstoffzusammensetzung nach Anspruch 5, wobei die basische Stickstoff-Verbindung ist: ein Carbonsäureamid, hergestellt aus einer oder mehr Carbonsäuren der Formel R2COOH, oder einem Derivat davon, das beim Umsetzen mit einem Amin ein Carbonsäureamid ergibt, wobei R2 C12-350-Alkyl oder C12-350-Alkenyl ist, und ein Kohlenwasserstoff-Polyamin.
  8. Treibstoffzusammensetzung nach Anspruch 7, wobei R2 C12-20-Alkyl oder C12-20-Alkenyl ist, und das Kohlenwasserstoff-Polyamin Tetraethylenpentamin oder Triethylentetramin ist.
  9. Treibstoffzusammensetzung nach Anspruch 5, wobei die basische Stickstoff-Verbindung eine Mannich-Base ist, hergestellt aus Dodecylphenol, Formaldehyd und Methylamin.
  10. Treibstoffzusammensetzung nach Anspruch 5, wobei die basische Stickstoff-Verbindung eine Mannich-Base ist, hergestellt aus C80-100-Alkylphenol, Formaldehyd und Triethylentetramin, Tetraethylenpentamin oder Gemischen davon.
  11. Treibstoffzusammensetzung nach Anspruch 1, wobei der polare Aktivator Wasser ist.
  12. Treibstoffzusammensetzung nach Anspruch 1, wobei das Carbonsäureamid der Komponente (2) hergeleitet ist von einer Carbonsäure der Formel R2COOH, wobei R2 C12-20-Alkyl ist, und einem Ethylenamin.
  13. Treibstoffzusammensetzung nach Anspruch 1, wobei das Succinimid der Komponente (3) hergeleitet ist von Polyisobutenyl-Bernsteinsäureanhydrid, wobei der Polyisobutenylrest 50 bis 250 Kohlenstoffatome enthält, und einem Ethylenamin.
  14. Treibstoffzusammensetzung nach Anspruch 1, wobei die Schmiermittelzusammensetzung 0,05 bis 15 Gew.% der molybdänhaltigen Zusammensetzung der Komponente (1), 0,05 bis 20 Gew.% des Carbonsäureamids der Komponente (2) und 0,05 bis 15 Gew.% des Succinimides der Komponente (3) enthält.
  15. Treibstoffzusammensetzung nach Anspruch 1, wobei der Molybdänkomplex mit der schwefelhaltigen Verbindung in einer Menge umgesetzt wird, die ausreicht, dass 2,0 bis 4,0 Schwefelatome pro Molybdänatom bereitgestellt werden.
  16. Treibstoffzusammensetzung nach Anspruch 15, wobei der Molybdänkomplex mit der schwefelhaltigen Verbindung in einer Menge umgesetzt wird, die ausreicht, dass 2,5 bis 4,0 Schwefelatome pro Molybdänatom bereitgestellt werden.
  17. Treibstoffzusammensetzung nach Anspruch 1, wobei die Additiv-Formulierung zudem einen Flockungsmittel-Inhibitor enthält.
  18. Treibstoffzusammensetzung nach Anspruch 17, wobei die Additiv-Formulierung zudem ein Schmiermittel enthält.
  19. Verfahren zur Verringerung von Motorablagerungen und Kolbenringblockierung in einem Zweitaktmotor, umfassend den Betrieb des Zweitaktmotors mit einer Treibstoffzusammensetzung, die eine größere Menge eines im Benzinbereich siedenden Treibstoffs und eine geringere Menge einer Schmiermittelzusammensetzung umfasst, umfassend:
    (A) eine größere Menge eines Basisöls mit Schmierviskosität, und
    (B) eine kleinere Menge einer Additiv-Formulierung, die die Verringerung von Motorablagerungen und Kolbenringblockierung bewirkt, umfassend:
    (1) 0,05 bis 15 Gew.% einer sulfurierten molybdänhaltigen Zusammensetzung, hergestellt durch (i) Umsetzen einer sauren Molybdänverbindung und einer basischen Stickstoffverbindung, ausgewählt aus der Gruppe mit einem Succinimid, einem Carbonsäureamid, einem Kohlenwasserstoffmonoamin, einem Kohlenwasserstoffpolyamin, einer Mannich-Base, einem Phosphoramid, einem Thiophosphoramid, einem Phosphonamid, oder einem Gemisch davon, in Gegenwart eines polaren Aktivators, so dass ein Molybdänkomplex entsteht, wobei 0,01 bis 2 Molybdänatome pro basischem Stickstoffatom zugegen sind, und der Aktivator im Verhältnis von 0,01 bis 50 Mol polarer Aktivator pro Mol Molybdän zugegen ist; und (ii) Umsetzen des Molybdänkomplexes mit einer schwefelhaltigen Verbindung in einer Menge, die ausreicht, dass 1,5 bis 4,0 Schwefelatome pro Molybdänatom bereitgestellt werden, wodurch eine schwefel- und molybdänhaltige Zusammensetzung entsteht,
    (2) 0,05 bis 20 Gew.% eines Carbonsäureamides, und
    (3) 0,05 bis 15 Gew.% eines Succinimides.
  20. Verfahren nach Anspruch 19, wobei die Schwefelquelle für Komponente (1) ist: Schwefel, Schwefelwasserstoff, Phosphorpentasulfid, R2Sx, wobei R Kohlenwasserstoff ist, und x mindestens 2 ist, anorganische Sulfide oder anorganische Polysulfide, Thioacetamid, Thioharnstoff, Mercaptane der Formel RSH, wobei R Kohlenwasserstoff ist, oder ein schwefelhaltiges Antioxidans.
  21. Verfahren nach Anspruch 20, wobei die Schwefelquelle für Komponente (1) ist: Schwefel, Schwefelwasserstoff, Phosphorpentasulfid, R2Sx, wobei R C1-4-Kohlenwasserstoff ist, und x mindestens 3 ist, anorganische Sulfide oder anorganische Polysulfide, Thioacetamid, Thioharnstoff, oder RSH, wobei R C1-40-Alkyl ist, und die saure Molybdänverbindung Molybdänsäure, Ammoniummolybdat oder Alkalimetallmolybdat ist.
  22. Verfahren nach Anspruch 21, wobei die Schwefelquelle Schwefel, Schwefelwasserstoff, RSH, wobei R C1-10-Alkyl ist, Phosphorpentasulfid oder (NH4)2Sx' ist, wobei x' mindestens 1 ist, die saure Molybdänverbindung Molybdänsäure oder Ammoniummolybdat ist, und die basische Stickstoffverbindung ein Succinimid, Carbonsäureamid oder eine Mannich-Base ist.
  23. Verfahren nach Anspruch 22, wobei die basische Stickstoffverbindung ein C24-350-Kohlenwasserstoff-Succinimid, ein Carbonsäureamid oder eine Mannich-Base ist, die aus einem C9-200-Alkylphenol, Formaldehyd und einem Amin hergestellt ist.
  24. Verfahren nach Anspruch 23, wobei die basische Stickstoff-Verbindung ein Polyisobutenyl-Succinimid ist, das hergestellt ist aus Polyisobutenyl-Bernsteinsäureanhydrid und Tetraethylenpentamin oder Triethylentetramin.
  25. Verfahren nach Anspruch 23, wobei die basische Stickstoff-Verbindung ist: ein Carbonsäureamid, hergestellt aus einer oder mehr Carbonsäuren der Formel R2COOH, oder einem Derivat davon, das beim Umsetzen mit einem Amin ein Carbonsäureamid ergibt, wobei R2 C12-350-Alkyl oder C12-350-Alkenyl ist, und ein Kohlenwasserstoff-Polyamin.
  26. Verfahren nach Anspruch 25, wobei R2 C12-20-Alkyl oder C12--20-Alkenyl ist, und das Kohlenwasserstoff-Polyamin Tetraethylenpentamin oder Triethylentetramin ist.
  27. Verfahren nach Anspruch 23, wobei die basische Stickstoff-Verbindung eine Mannich-Base ist, hergestellt aus Dodecylphenol, Formaldehyd und Methylamin.
  28. Verfahren nach Anspruch 23, wobei die basische Stickstoff-Verbindung eine Mannich-Base ist, hergestellt aus C80-100-Alkylphenol, Formaldehyd und Triethylentetramin, Tetraethylenpentamin oder Gemischen davon.
  29. Verfahren nach Anspruch 19, wobei der polare Aktivator Wasser ist.
  30. Verfahren nach Anspruch 19, wobei das Carbonsäureamid der Komponente (2) hergeleitet ist von einer Carbonsäure der Formel R2COOH, wobei R2 C12-20-Alkyl ist, und einem Ethylenamin.
  31. Verfahren nach Anspruch 19, wobei das Succinimid der Komponente (3) hergeleitet ist von Polyisobutenyl-Bernsteinsäureanhydrid, wobei der Polyisobutenylrest 50 bis 250 Kohlenstoffatome enthält, und einem Ethylenamin.
  32. Verfahren nach Anspruch 19, wobei die Schmiermittelzusammensetzung 0,05 bis 15 Gew.% der molybdänhaltigen Zusammensetzung der Komponente (1), 0,05 bis 20 Gew.% des Carbonsäureamids der Komponente (2) und 0,05 bis 15 Gew.% des Succinimides der Komponente (3) enthält.
  33. Verfahren nach Anspruch 19, wobei der Molybdänkomplex mit der schwefelhaltigen Verbindung in einer Menge umgesetzt wird, die ausreicht, dass 2,0 bis 4,0 Schwefelatome pro Molybdänatom bereitgestellt werden.
  34. Verfahren nach Anspruch 33, wobei der Molybdänkomplex mit der schwefelhaltigen Verbindung in einer Menge umgesetzt wird, die ausreicht, dass 2,5 bis 4,0 Schwefelatome pro Molybdänatom bereitgestellt werden.
  35. Verfahren nach Anspruch 19, wobei die Additiv-Formulierung zudem einen Flockungsmittel-Inhibitor enthält.
  36. Verfahren nach Anspruch 35, wobei die Additiv-Formulierung zudem ein Schmiermittel enthält.
EP93921434A 1992-09-11 1993-09-09 Brennstoffzusammensetzung für zweitaktmotoren Expired - Lifetime EP0616635B1 (de)

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EP0616635A1 (de) 1994-09-28
CA2122825A1 (en) 1994-03-31
WO1994006897A1 (en) 1994-03-31
AU4852593A (en) 1994-04-12
CA2122825C (en) 2003-12-30
DE69322952D1 (de) 1999-02-18
JPH07501360A (ja) 1995-02-09
AU670118B2 (en) 1996-07-04
US20020038525A1 (en) 2002-04-04
EP0616635A4 (de) 1995-02-22
DE69322952T2 (de) 1999-05-27
JP3495043B2 (ja) 2004-02-09

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