Classifications

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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M7/00—Solid or semi-solid compositions essentially based on lubricating components other than mineral lubricating oils or fatty oils and their use as lubricants; Use as lubricants of single solid or semi-solid substances
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  • C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
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  • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
  • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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  • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
  • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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  • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
  • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
  • C10M2203/108—Residual fractions, e.g. bright stocks
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  • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
  • C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/283—Esters of polyhydroxy compounds
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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  • C10M2207/286—Esters of polymerised unsaturated acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/30—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/34—Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
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  • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
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  • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
  • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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  • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
  • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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  • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
  • C10M2229/02—Unspecified siloxanes; Silicones
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  • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
  • C10M2229/04—Siloxanes with specific structure
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  • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
  • C10M2229/04—Siloxanes with specific structure
  • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
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  • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
  • C10M2229/04—Siloxanes with specific structure
  • C10M2229/043—Siloxanes with specific structure containing carbon-to-carbon double bonds
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
  • C10M2229/04—Siloxanes with specific structure
  • C10M2229/044—Siloxanes with specific structure containing silicon-to-hydrogen bonds
• • 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
  • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
  • C10M2229/04—Siloxanes with specific structure
  • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
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  • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
  • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
  • C10N2030/32—Light or X-ray resistance
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  • C10N2040/00—Specified use or application for which the lubricating composition is intended
  • C10N2040/02—Bearings
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  • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
  • C10N2050/10—Semi-solids; greasy
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  • C10N2060/00—Chemical after-treatment of the constituents of the lubricating composition
  • C10N2060/04—Oxidation, e.g. ozonisation

Definitions

• This invention relates to an improvement in grease compositions. More particularly, it relates to grease compositions having improved water resistance and resistance to deterioration in the presence of ionizing radiation.
• Grease compositions normally comprise a gelling agent dispersed in colloidal form in a lubricating oil base.
• Many types of gelling agents and of oil bases have been investigated. and utilized.
• the most widely employed greases are gelled with soaps of high molecular weight fatty acids and mineral lubricants are the most generally utilized oil base.
• greases gelled with soaps have certain inherent disadvantages which cannot be overcome by the use of additives or by other means than substitution of-the soaps.
• the soap-base greases for example, exhibit softening points at relatively moderate temperatures which are normally substantially below the decomposition temperature of either the soap or of the oil. This is due in large part to the relatively low melting point of the soap fibers dispersed in the oil.
• microgels comprise a large variety of colloidal substances which are either inorganic colloids or are organic derivatives of these colloids.
• Typical materials include silica, clays and the so-called onium clays as well as surface esterified colloids, such as butylated silica and the like.
• the greases prepared therefrom exhibit water sensitivity which limits their field of use.
• the onium clays and the surface esterified silica are waterproofed by surface treatments. In these cases the ester groups or the onium radicals perform a hydrophobing function, providing the colloids with an oleophilic surface which enables them to maintain their grease structure even in the presence of water.
• the hydrophobic surfactants normally utilized for improving the water resistance of greases gelled with inorganic colloids include particularly the cationic surfactants which may be amines and amino amides, preferably aliphatic in character and of relatively high molecular weight. While these improve the Water resistance of the colloidal gelled greases containing them, they do not prevent (in fact, they even accelerate) sensitivity of ice 2 the grease is made up of the cost of the individual ingredients. Consequently, any reduction in the cost of an essential ingredient correspondingly lowers the cost of the total grease composition and thereby improves the possible applicability of the grease to additional indus trial usage.
• the most expensive ingredient utilized in the microgel grease systems is the hydrophobing additive, since the gelling agent and the lubricant are in most instances relatively less costly.
• Th ehydrophobic surfactants are utilized for the sole reason that they are essential for the promotion of Water resistance of the 'grease compositions containing them.
• grease composition which exhibit excellent water resistance, have no dropping point and are stable in the presence of ionizing radiation while at the same time the cost of the composition is reduced.
• These compositions comprise a lubricating oil gelled to a grease consistency with an inorganic colloidal gelling agent, the agent bearing on the surface of the colloidally dispersed particles asphaltenes, as more fully defined hereinafter, in an of the grease to ionizing radiation.
• compositions comprise mineral oil bright stocks gelled to a grease consistency with colloidally dispersed clay, the clay bearing 25-100% by weight (based on. the clay) of oxidized asphaltenes.
• asphaltenes which are employed for the present purpose may be naturally occurring components obtained from petroleum residues as more fully described hereinafter, much better results are obtained if they have been subjected to an oxidizing treatment, preferably air blowing or other oxidation by means of oxygen-contain-. ing gas.
• asphaltenes is defined in Abraham, Asphalts and Allied Substances, Fifth Edition, pages 1165-6, as being the non-mineral constituents remaining insoluble in petroleum naphtha, thus differentiating them from the maltenes (petrolenes) which dissolve in the same medium and under the same conditions. As the test is run at room temperature (6 5-75 R), this latter constitutes a part of the definition. A still further limitation is the proportion of petroleum naphtha employed for the purpose of causing separation. I According to the standardized method, 50 volumes of petroleum naphtha are employed,;the test temperature normally being ambient room temperature. While this standard procedure defines the term, it will be understood that the asphaltic fraction insoluble at room temperature in any aliphatic hydrocarbon having 5-12 carbon atoms per molecule may be regarded as asphaltene for the purpose of the present invention.
• Asphaltenes may be isolated from other asphaltic constituents by preferential precipitation.
• asphalts may be introduced into an aliphatic hydrocarbon precipitant (C alkanes) by several alternative methods, dependent upon their physical characteristics.
• C alkanes aliphatic hydrocarbon precipitant
• hard asphalts especially cracked or blown having penetrations at 77 F. less than about 10 are preferably introduced by first dissolving them in a minimum amount
• the aromatic solvent is preferably one predominating in aromatic hydrocarbons having less than 10 carbon atoms per molecule, of which benzene, toluene and xylene are suitable members.
• Softer asphalts may be dispersed by refluxing in the presence of a limited proportion of the precipitating aliphatic hydrocarbon, although the aromatic solvent may be used in addition to or in place of the aliphatic medium.
• the maltene solution and precipitated particles are separated by any suitable means, including filtration, centrifuging, sedimentation, decanting or similar treatment.
• asphaltene particles may then be dissolved in an aromatic volatile solvent for use in the modification of microgel grease compositions. They may be added to such compositions under a variety of circumstances, such as by addition to an aqueous gel of the gelling agent or by dispersal in the lubricating oil prior to or subsequent to incorporation of the gelling agent in the oil.
• Asphaltene analysis It has been determined that asphaltenes are polycyclic, contain numerous hetero atoms, particularly nitrogen, sulfur and oxygen, and usually contain between 1 and 13 hetero atoms, usually 4-10, per asphaltene molecule on the average.
• the metallic content of asphaltenes is in the order of 0.1-0.3%, the major constituents being iron, vanadium, sodium and nickel.
• About A of the nitrogen atoms are weakly basic and only about 1% of the nitrogen atoms are strongly basic.
• Approximately of the sulfur groups exist as aliphatic or alicyclic sulfides, 1% as disulfides and 57% of the sulfur as thiophenes or polythiophenes.
• the asphaltenes may be oxidized either prior to or subsequent to their separation from other asphaltic components such as maltenes and the like. Oxidation results in the conversion of maltenes to asphaltenes, and the further polymerization of asphaltenes. Oxidation may be carried out by means well known in the asphalt art. For the most part, such operations are conducted by simply blowing the asphaltic body with air at an elevated temperature (450-550 F.) for an extended period of between about 1-15 hours. The oxidation may be carried out in the presence of oxidizing catalysts if desired, such as phosphoric acid, phosphorus pentoxide, ferric chloride, Friedel-Crafts catalyst, and the like'although this is not an essential feature of this invention.
• the isolated asphaltenes have been found to be especially sensitive to oxidation especially in the presence of ultraviolet light, such as sun light.
• lubricating oils which may be mineral lubricants, especially petroleum lubricating oils, as Well as synthetic lubricants, including esters, ethers, silicone fluids, and other well known materials.
• Specific lubricants include mineral oil bright stocks, methyl phenyl silicone fluids, dimethyl silicone fluids, polyphenyl ethers,-diesters of aliphatic dicarboxylic acids with monohydric alcohols, such as bis- (2-ethylhexyl)sebacate, polyesters, such as'pentaerythritol esters of C aliphatic monohydric alcohols, complex esters formed between polybasic aliphatic acids and polyhydric alcohols, and other materials well known for their lubricating properties.
• monohydric alcohols such as bis- (2-ethylhexyl)sebacate
• polyesters such as'pentaerythritol esters of C aliphatic monohydric alcohols, complex esters formed between polybasic aliphatic acids and polyhydric alcohols, and other materials well known for their lubricating properties.
• gas oil and waxy lubricant fractions distill over, leaving what is normally termed a short residue or a steam refined stock, also known as cylinder stock.
• the steam refined stock is then deasphalted (if an asphaltic crude is employed) and subjected to dewaxing operations to remove microcrystalline or macrocrystalline waxes.
• the oil is treated with a solvent for the purpose of reducing or removing the aromatic fractions.
• Clay contact treatment or percolation may be employed to clean up the oil following any one or all of these separate operations.
• the raflinate which remains after deasphalting, dewaxing, extraction, and clay treatment is generally called bright stock.
• the bright stocks suitable for use in the present compositions should have the following ranges of properties:
• Viscosity preferably 1500-3500 Viscosity, S.U.S., at 210 F, 75, usually -325, preferably -250 Viscosity index 60, preferably 85-110 Aniline point 100, preferably 115 Flash, F., 475, preferably 500 Fire, F., 550, preferably 600 Pour point, F., maximum 25, preferably lower than 15 Percent aromatics, 15, preferably 1 Percent naphthenes, 35
• Aerogels are normally prepared by forming TABLE II Examplesof typical bright stocks SUS Ring Analysis Aver- Vis- Average age cosity Rings 100 210 Index Aro- Naph- Paraf- Weight per matic thenes fins Mol Mid-Continent Bright Stock:
• the 8118210 F 0- 200-215 88 gels may be transferred into oil by the so-called direct Vlscoslty Index mmlmum' 90 9O transfer process wherein the hydrogel and oil are com- It will be understood from the above analyses that the source or treatment of a particular mineral oil is not as important for the present purpose as the final properties of the mineral oil constituent to be used in these compositions.
• the two most important properties of a mineral oil suitable for the present use comprise the aromatic content and the viscosity characteristics.
• the aromatic content has a large influence upon the sensitivity of the oil to thermal changes and the viscosity of the oils defines their suitability for their present purpose.
• the best definition with respect to essential characteristics of mineral oil suitable for the present compositions comprises those having a saturate molecule hydrocarbon content between about 15-65% and having a viscosity of between about 1250 and about 11,000 SUS at 100 F. Having defined these particular properties, the other properties such as flash, fire, aniline point, and viscosity index usually are largely dependent upon them.
• the gelling agents to be utilized in accordance with this invention include particularly the clays having relatively high base-exchange capacity, i.e., greater than milliequivalents per gram and preferably about 75-100 milliequivalents per gram.
• Bentonites such as Wyoming bentonite and hectorite as well as other montmorillonites are preferred.
• other inorganic colloids may be utilized, such as silica, magnesia, magnesia-silica, silica-alumina and other amorphous colloidal gels. They may be used in combination with clays or may constitute the sole gelling agent. Means are known for incorporating these classes of inorganic colloidal gels in lubricating oils for grease formation.
• Two of the favorite means comprise preparing the gels as aerogels which are low density gels bined, preferably in the presence of the asphaltenes, thus, causing separation of a major proportion of water from the gel, milling the remaining composition sufiiciently to disperse the gel throughout the oil and thereafter raising the temperature sufiiciently to eliminate the water remaining by evaporation.
• the greases ofthis invention are especially useful where the compositions are to be subjected to ionizing radiation since the asphaltenes absorbed on the surface of the gelling agent .act in some undetermined manner to maintain the consistency and properties of the grease.
• the greases are particularly useful for the lubrication of bearings and other relatively moving metallic surfaces which are exposed in atomic piles, atomic reactors, atomic powered machinery, such as in submarines and aircraft and for lubrication purposes generally where radiation is encountered.
• this special virtue does destrict the use of the grease to such locations since the greases are also highly satisfactory and effective for lubrication of bearings and other metallic surfaces where greases are generally required.
• microgel greases can normally be applied. Hence, they are especially useful for lubrication sites where high temperature or exposure to water will be encountered as well as in positions where ordinary operating conditions prevail.
• a grease composition was prepared by dispersing hectorite clay in a bright stock lubricating oil.
• the hectorite clay was modified by the presence of 60% by weight thereof of an amino amide hydrophobing agent.
• the grease contained 5% by weight of the clay.
• a second grease was prepared using the same bright stock lubricating oil to which was added a hectorite clay alcogel. After mixing, the alcohol was evaporated by heating, leaving the clay dispersed throughout the oil, A xylene solution of blown asphaltene was then added to the mixture and xylene evaporated, the components being milled thereafter to a. grease consistency.
• the grease contained 4% by weight of hectorite and 3% by weight of blown asphaltenes. These two greases were subjected to a high temperature and high speed bearing test using the Standard Federal Test Meth od No. 331 which requires a temperature of 300 F. and 10,000 r.p.m. The grease containing the amino amide ran for 562 hours until it failed, while the grease containing blown asphaltenes ran 378 hours until failure.
• the blown asphaltenes employed in the above comparative tests were obtained by air blowing a heavy crude lube residue having a 250 F. softening point and thereafter precipitating the asphalt with propane and extracting the asphaltenes by precipitation in isopentane.
• the asphaltenes had an average molecular weight (ebullioscopic) of 28,000.
• a grease composition consisting essentially of a lubricating oil gelled to a grease consistency with a grease forming proportion of a colloidally dispersed clay, said clay having absorbed on the surfaces thereof a hydrophobing amount of asphaltenes.
• a grease composition consisting essentially of a major proportion of a mineral lubricating oil and a minor proportion sufficient to thicken the oil to a grease consistency of a colloidally dispersed clay, said clay bearing on the surfaces thereof a minor amount, sufficient to increase the radiationand water-resistance of the grease, of asphaltenes.
• a grease composition consisting essentially of a major proportion of a mineral lubricating oil and a minor proportion, sufficient to impart a grease consistency to the composition of a colloidally dispersed bentonetic clay, said gel bearing on the surfaces thereof a minor amount, sufficient to increase the radiationand waterresistance of the grease, of oxidized asphaltenes.
• A' grease composition consisting essentially of a major proportion of a bright stock mineral oil gelled to a grease consistency with 1-15% by weight, based on the grease,of colloidally dispersed hectorite clay, said clay having adsorbed on the surfaces thereof 25-l00% by weight, based on the clay, of airblown asphaltenes.
• a grease composition consisting essentially of a major proportion of a polyphen-yl ether oil gelled to a grease consistency with 1-15 by weight of colloidally dispersed hectorite clay, said clay having absorbed on the surfaces thereof 25100% by weight, based on the clay, of airblown asphaltenes.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Organic Chemistry (AREA)
• Lubricants (AREA)

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Cited By (2)

Citations (3)

• 0
  • NL NL250416D patent/NL250416A/xx unknown
• 1959
  • 1959-04-13 US US805715A patent/US2981685A/en not_active Expired - Lifetime
• 1960
  • 1960-04-11 GB GB12815/60A patent/GB879896A/en not_active Expired
  • 1960-04-11 DE DES68012A patent/DE1101673B/de active Pending

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