US3705853A - Grease compositions - Google Patents

Grease compositions Download PDF

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Publication number
US3705853A
US3705853A US74849A US3705853DA US3705853A US 3705853 A US3705853 A US 3705853A US 74849 A US74849 A US 74849A US 3705853D A US3705853D A US 3705853DA US 3705853 A US3705853 A US 3705853A
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Prior art keywords
weight
grease
acids
terpolymer
acid
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US74849A
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Paul Fau
Richard J Petrucco
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ExxonMobil Oil Corp
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Mobil Oil Corp
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    • C10N2050/10—Semi-solids; greasy

Definitions

  • This invention relates to grease compositions and relates more particularly to grease compositions having improved resistance to water wash-out and resistance to softening at high temperature conditions.
  • grease compositions having improved resistance to water wash-out and resistance to softening at high temperature conditions, containing, as an improving agent, a minor amount sufi'icient to incorporate the aforementioned resistance, of an ethylene-vinyl ester-organic acid terpolymer, as more fully hereinafter described.
  • the terpolymers of the grease formulations of the present invention has a melt index of 0.5 to 200 and contain: (1) at least 65%, by Weight, of ethylene, (2) at least 5%, by weight, of a second ethylenically unsaturated monomer which is an ester of the group con- I sisting of the vinyl esters of the lower (16 carbon) satu rated aliphatic carboxylic acids; the alkyl acrylates, the alkyl methacrylates, the dialkyl maleates and the diaikyl fumarates of the lower (16 carbon) aliphatic alcohols; and (3) 0.01 to 3%, by weight, of a third ethylenically unsaturated monomer of the group consisting of acrylic, methacrylic, itaconic, maleic and fumaric acids; the anhydrides of itaconic, maleic and furnaric acids; the alkyl hydrogen maleates and the alkyl hydrogen fumarates; the monoacrylates and monomethacrylates of
  • thickening agents can be used in the greases of this invention. Included among the thickening agents are alkali and alkaline earth metal soaps of fatty acids and fatty materials having from about 12 to about 30 carbons atoms per molecule. The meals are typified by sodium, lithium, calcium and barium. Fatty materials are illustrated by stearic acid, hydroxystearic acid, stearin, cottonseed oil acids, oleic acid, palmitic acid, myristic acid and hydrogenated fish oils.
  • thickening agents include salt and salt-soap complexes as: calcium stearate-acetate (Pat. No. 2,197,263); barium stearate-acetate (Pat. No. 2,564,561); calcium stearate-caprylate-acetate complexes (Pat. No. 2,999,065); calcium caprylate-acetate (Pat. No. 2,999,066); and calcium salts and soaps of low-, intermediateand high molecular weight acids and of nut oil acids; and aluminum-complexes.
  • salt and salt-soap complexes as: calcium stearate-acetate (Pat. No. 2,197,263); barium stearate-acetate (Pat. No. 2,564,561); calcium stearate-caprylate-acetate complexes (Pat. No. 2,999,065); calcium caprylate-acetate (Pat. No. 2,999,066); and calcium salts and soaps of low-, intermediateand high mo
  • thickening agents comprise substituted ureas, phthalocyanines, indanthrene, pigments such as perylimides, pyromellitdiimides, ammeline, and carbon black.
  • thickening gelling agents employed in the new grease compositions are essentially hydrophobic clays.
  • Such thickening agents can be prepared from clays which are initially hydrophilic in character, but which have been converted into a hydrophobic condition by the introduction of long chain hydrocarbon radicals into the surface of the clay particles, prior to their use as a component of a grease composition, as, for example, by being subjected to a preliminary treatment with an organic cationic surface active agent, such as an onium compound.
  • Typical onium compounds are tetra alkyl ammonium chlorides, such as dimethyl dioctadecyl ammonium chloride, dimethyl dibenzyl ammonium chloride and mixtures thereof.
  • the clays which are useful as starting materials in forming the thickening agents to be employed in the grease compositions can comprise the naturally occurring chemically unmodified clays.
  • These clays are crystalline complex silicates, the exact composition of which is not subject to precise description, since they vary widely from one natural source to another.
  • These clays can be described as complex inorganic silicates such as aluminum silicates, magnesium silicates, barium silicates, and the like, containing, in addition to the silicate lattice, varying amounts of cation-exchangeable groups such as sodium.
  • Hydrophilic clays which are particularly useful for conversion to desired thickening agents include montmorillonite clays, such as bentonite, attapulgite, hectorite, illite, saponite, sepiolite, biotite, vermiculite, zeolite, clays and the like.
  • Preferred thickening agents are calcium leadacetate complexes employed in grease formulations as described in US. Pat. 2,898,297, issued Aug. 4, 1959.
  • Such thickening agents comprise a mixture of (A) alkaline earth metai soaps and salts therewith, the alkaline earth metals being selected from the group consisting of calcium and a mixture (B) of calcium and barium, not more than about 15% of barium on a chemical equivalent basis being associated in said mixture (B) with calcium in said soaps and salts, the mixture (A) of said soaps and salts being present in a grease-forming quantity, and the metal salts of said mixture (A) being salts of a low molecular weight unsubstituted saturated monocarboxylic acid (I) having from 1 to 6 carbon atoms per molecule, and the metal soaps of said mixture (A) being soaps of different acids with said acid (I) as shown in the following tabulation:
  • said acid (II) being selected from unsubstituted, monohydroxy--substituted and methyl-substituted saturated aliphatic monocarboxylic acids
  • acids (III) being selected from unsubstituted and monohydroxy-substituted saturated aliphatic monocarboxylic acids and monounsaturated aliphatic monocarboxylic acids
  • said oil acids being nut oil acids comprising mixtures of acids containing from about 8 to 18 carbon atoms per molecule and predominating in O -C acids; and from about 0.5 to about by weight (expressed as PbO) of at least one lead compound of at least one of said acids (1) through (IV).
  • Oils used in the greases of this invention can be mineral or synthetic oils of lubricating viscosity. Suitable mineral oils have a viscosity (SUS) of at least 40 seconds at 100 F., and particularly those within the range of about 60 seconds to about 6000 seconds at 100 F.
  • SUS viscosity
  • Synthetic vehicles can be used, instead of mineral oils, or in combination therewith.
  • Typical synthetic vehicles are: polypropylene, polypropylene glycol, trimethylol propane esters, neopentyl and pentaerythritol esters, di-(2- ethyl hexyl) sebacate, di(2-ethyl hexyl) adipate, dibutyl phthalate, polyethylene glycol di(2-ethyl hexoate), fluorocarbons perfiuoro-alkyl-polyethers, silicate esters, silanes, esters of phosphorus-containing acids, liquid ureas, ferrocene derivatives, hydrogenated mineral oils, chain type polyphenyls, siloxanes, and silicones (polysiloxanes) fluorosilicones, alkyl-substituted diphenyl ethers typified by a butyl-substituted bis-(
  • hydrocarbon oils include synthetic hydrocarbon polymers having improved viscosity indices, which polymers are prepared by polymerizing an olefin, or mixture of olefins, having from 5 to 18 carbon atoms per molecule in the presence of an aliphatic halide and a Ziegler-type catalyst.
  • compositions contemplated herein can also contain other characterizing materials.
  • antioxidants such as phenyl alphanaphthylamine (PAN), corrosion inhibitors, extreme pressure agents, viscosity index agents, and fillers can be used.
  • PAN phenyl alphanaphthylamine
  • Such materials are colloidal silica, calcium acetate, calcium carbonate and molybdenum disulfide.
  • Such characterizing materials do not detract from the lubricating value of the compositions of this invention, nor do they detract from the beneficial character of the terpolymers; rather, the characterizing materials serve to impart their customary properties to the particular compositions in which they are incorporated.
  • the greases of this invention can be prepared in accordance with conventional grease manufacturing procedures, as by any mixing technique wherein solid particles are wetted by a fluid.
  • Typical equipment for such use includes a colloid mill, 3-roll ink mill, Manton-Gaulin homogenizer and the like.
  • preferred terpolymers contain from about 20 to about by weight, of the aforementioned group (2) component, i.e. the second ethylenically unsaturated monomer component; and from about 0.1 to about 1%, by weight, of the aforementioned group (3) component, i.e. the third ethylenically unsaturated monomer component.
  • Representative preferred terpolymer comprise, in addition to ethylene, from about 20 to about 30% by weight, vinyl acetate and from about 0.1 to about 1%, by g y c aci from, about 20 to about 30%, y
  • the quantity of terpolymer improving agent is concerned, the latter, as previously indicated, is employed in a minor amount sufiicient to incorporate in the grease formulation the desired resistance to water washout and resistance to softening at high temperature conditions.
  • Particularly preferred are greases in which the terpolymer is present in an amount of at least about 0.01%, by weight, and for most purposes, the presence of the terpolymer in an amount from about 0.1 to about 5%, by weight, produces highly satisfactory improved grease compositions.
  • the thickener was formed by the reaction of a slight stoichiometric excess of metal base consisting of 4.5 parts of lime to 1 part litharge, with fatty acids comprising 27.5%, by weight, of a low molecular weight acid, viz acetic acid; 58%, by weight, of an intermediate molecular weight fatty acid, viz caprylic acid; and 14.5%, by Weight of high molecular Weight acids, viz coconut oil acids (C C).
  • the vehicle comprised a naphthenic solventrefined mineral oil stock of a viscosity of 800 SUS at F. and 70 SUS at 210 F.
  • the additives comprised 2%, by weight, of chlorinated wax as an extreme pressure agent; 0.8%, by weight, of antioxidants, viz hindered phenol and aromatic amine; and 1.2%, by weight, of corrosion inhibitors.
  • a typical representative terpolymer comprised an ethylene-vinyl acetate-methacrylic acid terpolymer, having a melt index of 13 and containing 27.5 by weight, vinyl acetate, 0.7%, by weight, methacrylic acid, and 71.8%, by weight, ethylene.
  • a grease composition as defined in claim 1 where- Table II the terpolymers of the present invention are highly effective in imparting resistance of the grease to softening at elevated temperatures.
  • a grease composition comprising a lubricating vehicle, a grease-forming quantity of a thickening agent and a minor effective amount of an improving agent comprising a terpolymer having a melt index of 0.5 to 200 and containing: (1) at least 65%, by Weight, of ethylene, (2) at least 5%, by weight, of a second ethylenically unsaturated monomer which is an ester of the group consisting of: the vinyl esters of saturated aliphatic carboxylic acids having 1-6 carbons; the alkyl acrylates, the alkyl methacrylates, the dialkyl maleates and the dialkyl fumarates of aliphatic alcohols having 16 carbons; and (3) 0.01 to 3.0%, by weight, of a third ethylenically unsaturated monomer of the group consisting of: acrylic, methacrylic, itaconic, maleic and fumaric acids; the anhydrides of itaconic, maleic and fumaric acids; the alkyl hydrogen maleates and the
  • a grease composition as defined in claim 1 wherein the terpolymer contains from about 20 to about 30%, by Weight, of the group (2) component and from about 0.1 to about 1%, by weight, of the group (3) monomer component.
  • a grease composition as defined in claim 1 wherein the terpolymer contains from about 20 to about 30%, by weight, methyl methacrylate and from about 0.1 to about 1%, by weight, methacrylic acid.
  • in the vehicle comprises a synthetic lubricating oil.
  • a grease composition as defined in claim I wherein the thickening agent comprises a mixture of (A) alkaline earth metal soaps and salts therewith, the alkaline earth metals being selected from the group consisting of calcium and a mixture (B) of calcium and barium, not more than about 15% of barium on a chemical equivalent basis being associated in said mixture (B) with calcium in said soaps and salts, the mixture (A) of said soaps and salts being present in a grease-forming quantity, and the metal salts of said mixture (A) being salts of a low molecular weight unsubstituted saturated monocarboxylic acid (I) having from 1 to 6 carbon atoms per molecule, and the metal soaps of said mixture (A) being soaps of different acids with said acid (I) as shown in the following tabulation:
  • said acid (II) being selected from unsubstituted, monohydroxy-substituted and methyl-substituted saturated aliphatic monocarboxylic acids, said acids (III) being selected from unsubstituted and monohydroxy-substituted saturated aliphatic monocarboxylic acids and monounsaturated aliphatic monocarboxylic acids; and said oil acids being nut oil acids comprising mixtures of acids containing from about 8 to 18 carbon atoms per molecule and predominating in C -C acids; and from about 0.5 to about 5%, by weight, expressed as PhD, of at least one lead compound of at least one of said acids (I) through (IV).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Organic Chemistry (AREA)
  • Lubricants (AREA)
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3904534A (en) * 1974-07-01 1975-09-09 Mobil Oil Corp Grease manufacture
US3997455A (en) * 1974-07-01 1976-12-14 Mobil Oil Corporation Paraffinic base greases
US4910246A (en) * 1984-06-11 1990-03-20 The Dow Chemical Company Intercalations of crystalline lithium aluminates
EP0359466A1 (de) * 1988-09-08 1990-03-21 Exxon Research And Engineering Company Schmiermittelgemisch
US5116522A (en) * 1988-09-08 1992-05-26 Exxon Research And Engineering Company Grease composition containing an ethylene copolymer having a melt index of at least about 40
WO2005028525A2 (de) * 2003-09-19 2005-03-31 Basf Aktiengesellschaft Amidgruppenhaltige ethylenterpolymere und ihre verwendung
US20050209114A1 (en) * 2004-03-19 2005-09-22 The Lubrizol Corporation, A Corporation Of The State Of Ohio Functionalized polymer composition for grease
WO2005108532A1 (de) * 2004-04-30 2005-11-17 Rohmax Additives Gmbh Schmierfett mit hoher wasserresistenz

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2205570B1 (de) * 1972-11-07 1976-06-04 Mobil Oil France
DE3136931A1 (de) * 1981-09-17 1983-04-07 Akzo Gmbh, 5600 Wuppertal Copolymere aus (alpha)-(beta)-ungesaettigten dicarbonsaeureestern, verfahren zu deren herstellung sowie deren verwendung als gleitmittel fuer die kunststoffverarbeitung
JPS59150579U (ja) * 1983-03-23 1984-10-08 大金興業株式会社 浄化槽流出水の蒸発散処理装置
US4606183A (en) * 1984-11-20 1986-08-19 Amsted Industries Incorporated Lubricated and thermoplastic impregnated wire rope
GB8503382D0 (en) * 1985-02-09 1985-03-13 British Petroleum Co Plc Lubricating grease

Family Cites Families (7)

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Publication number Priority date Publication date Assignee Title
US2698298A (en) * 1951-03-15 1954-12-28 Socony Vacuum Oil Co Inc Lubricating greases containing an acidic copolymer salt
US2698299A (en) * 1951-11-27 1954-12-28 Socony Vacuum Oil Co Inc Modified acidic copolymer-fatty acid soap greases
FR1226563A (fr) * 1959-02-20 1960-07-13 Exxon Standard Sa Graisses améliorées
US3086942A (en) * 1960-02-01 1963-04-23 Exxon Research Engineering Co Lubricants containing various crosslinked substances as thickening agents
US3076764A (en) * 1960-09-30 1963-02-05 California Research Corp Isotactic polymers of 4-methyl-1-pentene as grease thickeners
US3114708A (en) * 1960-12-29 1963-12-17 Exxon Research Engineering Co Dry polyolefin/oil blends
US3290244A (en) * 1963-07-11 1966-12-06 Sun Oil Co Grease compositions containing atactic polypropylene

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3904534A (en) * 1974-07-01 1975-09-09 Mobil Oil Corp Grease manufacture
JPS5124604A (de) * 1974-07-01 1976-02-28 Mobil Oil
US3997455A (en) * 1974-07-01 1976-12-14 Mobil Oil Corporation Paraffinic base greases
JPS5925836B2 (ja) * 1974-07-01 1984-06-21 モ−ビル オイル コ−ポレ−ション 潤滑グリ−スおよびその製法
US4910246A (en) * 1984-06-11 1990-03-20 The Dow Chemical Company Intercalations of crystalline lithium aluminates
EP0359466A1 (de) * 1988-09-08 1990-03-21 Exxon Research And Engineering Company Schmiermittelgemisch
US5116522A (en) * 1988-09-08 1992-05-26 Exxon Research And Engineering Company Grease composition containing an ethylene copolymer having a melt index of at least about 40
WO2005028525A2 (de) * 2003-09-19 2005-03-31 Basf Aktiengesellschaft Amidgruppenhaltige ethylenterpolymere und ihre verwendung
WO2005028525A3 (de) * 2003-09-19 2005-08-11 Basf Ag Amidgruppenhaltige ethylenterpolymere und ihre verwendung
US20050209114A1 (en) * 2004-03-19 2005-09-22 The Lubrizol Corporation, A Corporation Of The State Of Ohio Functionalized polymer composition for grease
WO2005090531A1 (en) * 2004-03-19 2005-09-29 The Lubrizol Corporation Functionalized polymer composition for grease
WO2005108532A1 (de) * 2004-04-30 2005-11-17 Rohmax Additives Gmbh Schmierfett mit hoher wasserresistenz
CN100552008C (zh) * 2004-04-30 2009-10-21 罗麦斯添加剂有限公司 具有高耐水性的润滑脂

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DE2143848B2 (de) 1981-07-23
FR2107892A1 (de) 1972-05-12
CA948616A (en) 1974-06-04
DE2143848A1 (de) 1972-03-30
GB1306349A (de) 1973-02-07
DE2143848C3 (de) 1982-04-29
AU3332971A (en) 1973-03-29
JPS5521079B1 (de) 1980-06-06
FR2107892B1 (de) 1976-03-26

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