US3809649A - Lubricating grease - Google Patents

Lubricating grease Download PDF

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Publication number
US3809649A
US3809649A US00327786A US32778673A US3809649A US 3809649 A US3809649 A US 3809649A US 00327786 A US00327786 A US 00327786A US 32778673 A US32778673 A US 32778673A US 3809649 A US3809649 A US 3809649A
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Prior art keywords
polyethylene
grease
weight
emulsion
greases
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US00327786A
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English (en)
Inventor
Doorne G Van
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Labofina SA
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Labofina SA
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • C—CHEMISTRY; METALLURGY
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02—Water
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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
    • C—CHEMISTRY; METALLURGY
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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
    • C10M2203/102—Aliphatic fractions
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/104—Aromatic fractions
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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
    • C10M2203/106—Naphthenic fractions
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/022—Ethene
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    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/06—Groups 3 or 13
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • Lubricating greases comprising 5 to 25% by weight, based on the weight of the greases, of thickening metal soap, 1 to by weight of an anionic emulsion of unoxidized polyethylene having a mean molecular weight higher than 10,000, said emulsion having a polyethylene content ranging from 35 to 60% and a metal sulfonate anionic emulsifier content ranging from 8 to 12% based on the weight of the emulsion, the means size of the polyethylene particles being comprised between 0.02 and 0.5 micron, the rest of the composition being an oleaginous vehicle containing usual additives for lubricating greases.
  • This invention relates to lubricating greases and more particularly to homogeneous greases with improved mechanical and chemical stability characteristics.
  • lubricating greases generally have been prepared from a lubricating base oil or oleaginous vehicle and a thickening agent which imparts the desired consistency to the grease.
  • Thickening agents most often employed are soaps of fatty acids or inorganic components, such as colloidal silica, bentonite, and the like.
  • the known greases are gels, the thickening agent forming a network wherein the oil is incorporated.
  • difiiculties are encountered for manufacturing homogeneous and stable gels, due to many factors, such as type of thickening agent, type of base oil, the amounts of such components, the process for manufacturing the grease, etc.
  • Greases containing these complexes are expensive and moreover they are not satisfactory for good lubricating performance.
  • lubricating greases containing ethylene polymers are not sufiiciently stable and tend to break under mechanical stresses with formation of a too fluid product (U.S.'
  • a further object of this invention is to provide homogeneous and consistent lubricating greases.
  • the present invention which fulfills these and other objects is a lubricating grease comprising 5 to 25% by weight, based on the total weight of the grease, of thickening soap, 1 to 10% by weight of an anionic emulsion of unoxidized polyethylene having a mean molecular weight higher than 10,000, said emulsion having a polyethylene content ranging from 35 to 60% and an anionic emulsifier content ranging from 8 to 12% based on the weight of the emulsion, the mean size of the polyethylene particles being between 0.02 and 0.5 micron, and the rest of the lubricating grease being an oleaginous vehicle containing conventional additives for lubricating greases.
  • the polyethylene emulsions of the present invention are prepared according to processes described in US. Pats. 3,296,162 and 3,352,807. These emulsions are prepared by free-radical polymerization of ethylene in an aqueous medium containing a mixture of anionic emulsifying agents. The emulsions so obtained are then stabilized by a post-treatment which comprises covering substantially of the surface of the particles with an anionic emulsifying agent. With these stabilized polyethylene emulsions, the total content of emulsifying agent depends primarily upon the size of the polymer particles.
  • the content of emulsifying agent may be about 10% by weight when the particles contain 40% of solid material with a particle size of about 0.03 micron, whereas this content may be only 8% by weight when such particle size is about 0.5 micron.
  • the content of emulsifying agent does not exceed 12% based on the weight of polymer emulsion, although higher contents could be used but without substantial improvement of the mechanical properties of the emulsions.
  • the stabilizing post-treatment is carried out with anionic compounds which are free from acidic groups.
  • the pH of the stabilized emulsions generally is higher than 8.
  • the stabilized polyethylene emulsions used in the present invention are quite different from the emulsions prepared from oxidized polyethylenes which generally have a relatively low molecular weight, usually lower than 5,000 and more often about 3,000.
  • the molecular weight is in part set by the methods by which emulsions are prepared from the emulsifiable polyethylene solids.
  • the mechanical properties of the polymers generally depend upon their molecular weight.
  • the emulsions of oxidized polyethylenes normally do not contain more than 20 to 30% of solid materials.
  • emulsions of unoxidized polyethylenes which are used in the lubricating greases of the present invention are quite different from the emulsions of oxidized polyethylenes, not only because of the higher content of polyethylene with a high molecular weight, higher than 10,000 and in the form of small particle sizes, but also because the pH of the unoxidized polyethylene is higher than 8 and gen erally, ranges between 8.5 and 10.
  • the polyethylene emulsions of the present in- 3 vention have an anionic emulsifying agent content of higher than 8%.
  • the lubricating greases of the present invention most commonly employed generally contain from 1 to 10% by weight of stabilized emulsion of unoxidized polyethylene in admixture with to 25% by weight of soap, the rest of the grease being an oleaginous vehicle containing conventional additives for lubricating greases.
  • a substantial improvement in the performance of the lubricating greases is obtained with a content in polyethylene emulsions as low as 1% by weight.
  • lubricating greases were prepared from naphthenic oil (SSU viscosity at 100 F.: 500) containing 8.5% by weight (based on the grease) of lithium 12-hydroxystearate, 0.5% of antioxydizing agent and 0.5 of rust-inhibiting agent.
  • One of the greases was prepared without adding polyethylene emulsion, while other greases (designated Greases B, C and D) were prepared containing respectively 1%, 2% and 3% of stabilized anionic emulsion of unoxidized polyethylene (Poly-Em 12, a product of Cosden Oil & Chemical Company).
  • the main characteristics of the polyethylene emulsion were:
  • Grease consistency by penetration test method ASTM D217 penetration is measured by the distance (in tenths millimeters) a standard cone will penetrate by free fall at 25 C. the surface of the grease placed in a cup. When the grease is merely placed in the cup, the penetration is reported as unworked. The unworked penetration of a grease being not always a suitable indication, the test is also carried out when the grease is worked in the worker cup (60 strokes in the present cast).
  • Water resistance test method ASTM D1264 the grease is water washed at controlled temperature and speed. The weight loss of grease is determined and calculated in weight pourcentage.
  • the improvement in properties ofthe grease is substantial even with a content of polyethylene emulsion of 1% based on the total weight of the composition, and is particularly noticeable when the content is in the range of 2 to 3% by weight.
  • the amount of stabilized emulsion of unoxidized polyethylene which is employed to improve the properties of the greases may be varied depending on the type of oleaginous vehicle and on the type of and amount of soap. With emulsion contents higher than 10%, the improvement does not justify the additional expense of the added emulsion. Therefore, as a practical matter, the content of polyethylene emulsion generally does not exceed 10% and is most often employed in amounts of between about 1 and 5% by weight.
  • the oleaginous vehicle employed advantageously is an aromatic or naphthenic oil, more particularly, a highly naphthenic oil which leads to greases with a better thermal stability.
  • Synthetic lubricating oils containing primarily sebacic or adipic esters of alcohols containing from 6 to 12 carbon atoms, such as 2-ethylhexanol, may be employed.
  • mineral oils or mixtures of mineral oils and a lesser amount of synthetic oil are economically more advantageous.
  • the amount of soap used as thickening agent generally is between 5 and 25% of the Weight of the grease, this percentage depending on the type of soap, the amount of polyethylene, the desired degree of consistency, and like considerations.
  • the soap employed may be virtually any of those commonly employed in lubricating greases.
  • the soap preferably is one prepared from a higher aliphatic carboxylic acid, saturated or unsaturated, containing from 12 to 18 carbon atoms, such as stearic, 12-hydroxystearic, palmitic, oleic acids, and the like.
  • Mixed soaps also may be used, these products being a mixture of two different soaps, such as a mixture of an alkaline soap and an aluminum soap.
  • Other valuable thickening agents are complex soaps prepared from a higher aliphatic carboxylic acid and a low molecular weight acid, such as soaps of benzostearic, acetopalmitic or toluostearic acids.
  • the greases of the present invention also may include any of the usual additives, such as anti-oxidizing agents, rust-preventive agents and extreme-pressure additives.
  • Particularly active anti-oxidizing agents are N-alkyl-paraphenylenediamines, naphthylamines and diand tri-alkylphenols.
  • Rust-preventive agents useful include primary amines containing from 6 to 18 carbon atoms or N-heterocyclized derivatives.
  • Extreme-pressure additives are generally selected from the group comprising arylphosphites, arylphosphates and arylthiophosphates, arylsulfides, sulfurized fatty oils, chlorinated parafiins, and the like.
  • Antiwear additives for example urea or thiourea derivatives, or some polyisobutylenes with a molecular weight higher than 800, acting as viscosity improvers, may also be added to the lubricating greases of the present invention. These additives may be employed in an amount which may vary between 0.1 and 10% by weight, more generally, between 1 and 5% based on the weight of the grease.
  • a homogeneous mixture of oleaginous vehicle and soap for preparing the lubricating greases of the present invention, known techniques may be used in carrying out the present process. Such process includes forming at a relatively high temperature, a homogeneous mixture of oleaginous vehicle and soap, adding the stabilized emulsion of polyethylene, cooling the mixture to form a gel and homogenizing this gel to obtain the desired structure.
  • EXAMPLE 1 This example illustrates the synergistic effect between the soap and the emulsion of polyethylene.
  • a lubricating grease consisting of 85.5% by weight of naphthenic oil (500 SSU at 100 F.), 14% of sodium soap of stearic acid and 0.5% of anti-oxidizing agent was found to have a penetration (60 strokes) of 266.
  • This grease was homogeneous, smooth and hard. Moreover, its mechanical stability was good. From penetration tests, the difference between the penetration at 60 strokes and 10,000 strokes (respectively 276 and 285) was very small.
  • the loss by water washing was 4.5% by weight.
  • Example 3 The grease of Example 3 was duplicated, but with the use of a mixed soap. This grease contained 5% by weight of lithium 12-hydroxystearate and 1.5% by weight of aluminum stearate.
  • This grease has a penetration of 261 (at 60 strokes).
  • This grease has a penetration (at 60 strokes) of 285 and a loss by water washing (at C.) of 1.4.
  • This grease is particularly consistent, the penetration (at 60 strokes) being 207.
  • a lubricating grease was prepared from 87.5% of mineral oil (500 SSU at 100 F.), 8.5% of lithium 12-hydroxystearate, 1% of usual additives and 3% of an unstabilized emulsion of polyethylene having a pH of 7.7 and a content of anionic emulsifying agent of 5.21%.
  • This grease had a penetration (at 60 strokes) of 312, a bleeding (or oil separation) index of 3.5 and a loss by water washing (at 80 C.) of 15%.
  • a grease similar with the above Grease D of the table, but prepared with the use of an emulsion of oxidized polyethylene was found to have poor mechanical stability, lumps being formed as a result of a breakdown of the emulsion and a coagulation of the polymer particles.
  • Lubricating greases comprising 5 to 25% by weight, based on the weight of the greases, of thickening metal soap; 1 to 10% by weight of an anionic emulsion of unoxidized polyethylene having a mean molecular weight higher than 10,000, said emulsion having a polyethylene content ranging from 35 to 60% and a metal sulfonate anionic emulsifier content ranging from 8 to 12% based 7 on the weight of the emulsion, the mean size of the polyethylene particles being comprised bet-ween 0.02 and ,0.5 micron, the rest of the composition being an oleaginous vehicle containing usual additives for lubricating greases.
  • the grease of claim 1 wherein the thickening soap is one prepared from a higher aliphatic carboxylic acid containing from 12 to 18 carbon atoms.
  • the grease of claim 3 wherein the thickening soap is one prepared from an acid selected from the group consisting of stearic, hydroxystearic, palmitic and oleicr 5.

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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)
US00327786A 1972-03-15 1973-01-29 Lubricating grease Expired - Lifetime US3809649A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BE115079A BE780687A (fr) 1972-03-15 1972-03-15 Graisses lubrifiantes.

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US3809649A true US3809649A (en) 1974-05-07

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US (1) US3809649A (de)
JP (1) JPS5143554B2 (de)
AU (1) AU466520B2 (de)
BE (1) BE780687A (de)
CA (1) CA991164A (de)
CH (1) CH560755A5 (de)
CS (1) CS172382B2 (de)
DE (1) DE2310590B2 (de)
FR (1) FR2175728B1 (de)
GB (1) GB1400020A (de)
IT (1) IT971063B (de)
NL (1) NL152927B (de)
NO (1) NO135095C (de)
SE (1) SE389126B (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3935122A (en) * 1975-04-01 1976-01-27 Mobil Oil Corporation Grease compositions
US4079013A (en) * 1975-10-17 1978-03-14 Mobil Oil Corporation Grease thickeners
US4283293A (en) * 1978-08-07 1981-08-11 Mobil Oil Corporation Metal working lubricant compositions
CN114606044A (zh) * 2022-03-22 2022-06-10 姚文兵 一种极压润滑脂及其制备方法
US11440875B2 (en) * 2017-03-31 2022-09-13 Daikin Industries, Ltd. Sulfonic acid, carboxylic acid, and salts thereof

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54132071A (en) * 1978-04-05 1979-10-13 Ntn Toyo Bearing Co Ltd Lubrication constituent for roller bearings
JPS55137198A (en) * 1979-04-13 1980-10-25 Ntn Toyo Bearing Co Ltd Lubricating composition for ball-and-roller bearing
DE3485789T2 (de) * 1984-02-06 1992-12-24 Mobil Oil Corp Fettzusammensetzung.
CA1280738C (en) * 1984-03-07 1991-02-26 Andrew Gene Horodysky Grease composition containing boron compound and hydroxy containing soap thickener
US5084194A (en) * 1984-03-07 1992-01-28 Mobil Oil Corporation Grease composition
US4780227A (en) * 1984-08-22 1988-10-25 Mobil Oil Corporation Grease composition containing borated alkoxylated alcohols
US4828734A (en) * 1985-08-27 1989-05-09 Mobil Oil Corporation Grease compositions containing borated oxazoline compounds and hydroxy-containing soap thickeners
JP2795767B2 (ja) * 1991-12-27 1998-09-10 株式会社東海理化電機製作所 摺動接点用グリース
US5845425A (en) * 1994-11-07 1998-12-08 Leake; Michael J. Photoframe and gift card combination

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3935122A (en) * 1975-04-01 1976-01-27 Mobil Oil Corporation Grease compositions
US4079013A (en) * 1975-10-17 1978-03-14 Mobil Oil Corporation Grease thickeners
US4283293A (en) * 1978-08-07 1981-08-11 Mobil Oil Corporation Metal working lubricant compositions
US11440875B2 (en) * 2017-03-31 2022-09-13 Daikin Industries, Ltd. Sulfonic acid, carboxylic acid, and salts thereof
CN114606044A (zh) * 2022-03-22 2022-06-10 姚文兵 一种极压润滑脂及其制备方法

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BE780687A (fr) 1972-07-03
GB1400020A (en) 1975-07-16
NL7216781A (de) 1973-09-18
JPS491959A (de) 1974-01-09
FR2175728B1 (de) 1976-06-04
NO135095C (de) 1977-02-09
CS172382B2 (de) 1976-12-29
NO135095B (de) 1976-11-01
CH560755A5 (de) 1975-04-15
AU5228473A (en) 1974-08-22
NL152927B (nl) 1977-04-15
JPS5143554B2 (de) 1976-11-22
DE2310590A1 (de) 1973-09-20
DE2310590B2 (de) 1978-08-31
SE389126B (sv) 1976-10-25
CA991164A (en) 1976-06-15
AU466520B2 (en) 1975-10-30
IT971063B (it) 1974-04-30
FR2175728A1 (de) 1973-10-26

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