US3904534A - Grease manufacture - Google Patents

Grease manufacture Download PDF

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Publication number
US3904534A
US3904534A US484909A US48490974A US3904534A US 3904534 A US3904534 A US 3904534A US 484909 A US484909 A US 484909A US 48490974 A US48490974 A US 48490974A US 3904534 A US3904534 A US 3904534A
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United States
Prior art keywords
weight
percent
terpolymer
grease
group
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US484909A
Inventor
Francis S Sayles
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ExxonMobil Oil Corp
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Mobil Oil Corp
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Publication date
Application filed by Mobil Oil Corp filed Critical Mobil Oil Corp
Priority to US484909A priority Critical patent/US3904534A/en
Priority to ZA4010A priority patent/ZA754010B/en
Priority to GB13087/76A priority patent/GB1507698A/en
Priority to GB26946/75A priority patent/GB1507697A/en
Priority to US05/590,760 priority patent/US3997455A/en
Priority to DE2560382A priority patent/DE2560382C2/en
Priority to DE2528600A priority patent/DE2528600C2/en
Priority to CA230,533A priority patent/CA1050524A/en
Priority to AU82594/75A priority patent/AU497712B2/en
Priority to FR7520669A priority patent/FR2277143A1/en
Priority to JP50080576A priority patent/JPS5925836B2/en
Application granted granted Critical
Publication of US3904534A publication Critical patent/US3904534A/en
Priority to JP55085270A priority patent/JPS6019954B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/022—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amino group
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    • C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
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    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
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    • 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
    • C10M2227/02—Esters of silicic acids
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    • 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
    • C10M2227/08—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 having metal-to-carbon bonds
    • C10M2227/081—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 having metal-to-carbon bonds with a metal carbon bond belonging to a ring, e.g. ferocene
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    • C10M2229/02—Unspecified siloxanes; Silicones
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    • 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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    • 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
    • C10M2229/051—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing halogen
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    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
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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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    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • ABSTRACT In a process for manufacturing a calcium complex [52] US Cl 252/36; 252/40.5; 252/5 l .5 R; grease in which there is incorporated an ethylene-vinyl 252/5l.5 A; 252/56 R esterorganic acid terpolymer as an improving agent, a [5] Int. Cl.
  • ClOm 5/16; ClO 5/12 method is provided for improving grease formulation, [58] Field of Search 252/36, 5 l .5 R, 51.5 A, obtaining improved yield and making use of previously 252/56 R, 40.5 unsuitable oils by introducing the terpolymer to the charge of the lubricating vehicle and thickening agent [5 6] References Cited components prior to saponification.
  • This invention relates to grease manufacture and, in one of its aspects, relates more particularly to a process for manufacturing a calcium complex grease in which there is incorporated in the formulation an ethylenevinyl ester-organic acid terpolymer for improving water wash-out resistance and resistance to softening at relatively high temperature environments.
  • the terpolymers of these formulations have a melt index of 0.5 to 200 and contain: l at least 65 percent, by weight, of ethylene, (2) at least 5 percent, by weight, of a second ethyleneically unsaturated monomer which is an ester of the group consisting of the vinyl esters of the lower (1-6 carbon) saturated aliphatic carboxylic acids, the alkyl acrylates, the alkyl methacrylates, the dialkyl maleates and the dialkyl fumarates of the lower l6 carbon) aliphatic alcohols; and (3) 0.01 to 3 percent, 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 alkyl hydrogen fumarates; the monoacrylates and monomethylacrylates of glycols', 2-hydroxy-3-aminopropyl
  • the thickening agents employed in the greases of the present invention comprise calcium complex soaps, including calcium acetate complex soaps and calcium lead acetate complex soaps.
  • Oils used in the greases of this invention can be min eral or synthetic oils of lubricating viscosity.
  • Suitable mineral oils have a viscosity (SUS) of at least 40 seconds at 100F, and particularly those within the range of about 60 seconds to about 6,000 seconds at 100F.
  • 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 pentacrythritol esters, di(2-ethyl hexyl) sebacate, di-(2-ethyl hexyl) adipate, dibutyl phthalate, polyethylene glycol di(2- atoms per molecule in the presence of an aliphatic halide and a Zielger-type catalyst.
  • preferred terpolymers contain from about 20 to about 30 percent, by weight, of the aforementioned group (2) component, i.e. the second ethylenically unsaturated monomer component; and from about 0.1 to about 1 percent, by weight, of the aforementioned group (3) component, i.e. the third ethylenically unsaturated monomer component.
  • Representative preferred terpolymers comprise, in addition to ethylene, from about 20 to about 30 percent, by weight, vinyl acetate and from about 0.1 to about 1 percent, by weight, acrylic acid; from about 20 to about 30 percent, by weight, vinyl acetate and from about 0.1 to about l%, by weight, methacrylic acid; from about 20 to about 30 percent, by weight, ethyl acrylate and from about 0.1 to about 1 percent, by weight, acrylic acid; from about 20 to about 30 percent, by weight, ethyl acrylate and from about 0.
  • terpolymer improving agent insofar as the quantity of terpolymer improving agent is concerned, the latter as previously indicated, is employed in a minor amount sufficient to incorporate in the grease formulation the desired resistance to Water wash-out 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 percent, by weight, and for most purposes, the presence of the terpolymer in an amount from about 0.] to about 5 percent, by weight, produces highly satisfactory improved grease compositions.
  • the terpolymer contains from about 20 to about 30 percent, by weight, of the group (2) monomer component and from about 0.1 to about 1 percent, by weight, of the group (3) monomer component.
  • a particularly preferred terpolymer is one having a melt index of about 6 and containing about 71.8 percent, by weight, ethylene, about 25 percent, by weight, vinyl acetate and about 0.7 percent, by weight, methacrylic acid.
  • the terpolymer was added at this point, in other examples it constituted a part of the orginal charge to the contactor. In the former cases dehydration of the soap base is concurrent with dispersion of the terpolymer therein. Cooling, addition of various additive packages, homoginization and final addition of oil, complete the manufacture.
  • the terpolymer employed in the examples of Tables I and II had a melt index of about 6 and contained about 71.8 percent, by weight, ethylene, about percent, by weight, vinyl acetate and about 0.71 percent, by weight, methacrylic acid.
  • the base oils employed in the examples of Table I comprised either a 500 SUS solvent naphthenic neutral oil, with a V.l.
  • the base oils employed in the examples of Table II comprised either a 900 SUS solvent naphthenic neutral oil having a V.I. of 65 or a 300 SUS solvent paraffinic neutral oil having a ⁇ /.l. of 90.
  • said grease composition comprises 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: l at least 65 percent, by weight, of ethylene, (2) at least 5 percent, 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 l6 carbons; the alkyl acrylatcs, the alkyl methacrylates, the dialkyl maleates and the dialkyl fumarates of aliphatic alchols having 1-6 carbons; and (3) 0.0l to 3 percent, 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
  • the terpolymer contains from about 20 to about 30 percent, by weight, of the group (2) component and from about 0.1 to about 1 percent, by weight, of the group (3) monomer component.
  • terpolymer contains from about 20 to about 30 percent, by weight, of vinyl acetate and from 0.1 to about 1 percent, by weight, acrylic acid.
  • terpolymer contains from about 20 to about 30 percent, by weight, ethylacrylate and from about 0. l to about 1 percent, by weight, methacrylic acid.
  • terpolymer contains from about 20 to about 30 percent, by weight, methylmethacrylate and from about 0.1 to about 1 percent, by weight, mcthacrylic acid.

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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)

Abstract

In a process for manufacturing a calcium complex grease in which there is incorporated an ethylene-vinyl esterorganic acid terpolymer as an improving agent, a method is provided for improving grease formulation, obtaining improved yield and making use of previously unsuitable oils by introducing the terpolymer to the charge of the lubricating vehicle and thickening agent components prior to saponification.

Description

United States Patent [19 Sayles Sept. 9, 1975 GREASE MANUFACTURE [75] inventor: Francis S. Sayles, Rocky Hill, NJ. Primary Examnfer Delbefl Gamz Asszstanl Exammerl. Vaughn [7 As g'n l M il Oil Corporation, New York, Attorney, Agent, or Firm-Charles A Huggett; Oswald NY. G. Hayes [22] Filed: July 1, 1974 [21 1 App]. No.: 484,909 [57] ABSTRACT In a process for manufacturing a calcium complex [52] US Cl 252/36; 252/40.5; 252/5 l .5 R; grease in which there is incorporated an ethylene-vinyl 252/5l.5 A; 252/56 R esterorganic acid terpolymer as an improving agent, a [5] Int. Cl. ClOm 5/16; ClO 5/12 method is provided for improving grease formulation, [58] Field of Search 252/36, 5 l .5 R, 51.5 A, obtaining improved yield and making use of previously 252/56 R, 40.5 unsuitable oils by introducing the terpolymer to the charge of the lubricating vehicle and thickening agent [5 6] References Cited components prior to saponification.
UNITED STATES PATENTS 15 Claims, N0 Drawings 3,705,853 12/1972 Fran et al. 252/36 GREASE MANUFACTURE BACKGROUND OF THE INVENTION 1. Field of the Invention This invention relates to grease manufacture and, in one of its aspects, relates more particularly to a process for manufacturing a calcium complex grease in which there is incorporated in the formulation an ethylenevinyl ester-organic acid terpolymer for improving water wash-out resistance and resistance to softening at relatively high temperature environments.
2. Description of the Prior Art In commonly assigned US. Pat. No. 3,705,853, issued Dec. 12, 1972, there are provided grease compositions having improved resistance to water wash-out and resistance to softening at high temperature conditions, comprising calcium complex greases containing ethylene-vinyl ester organic acid terpolymers as improving agents. More specifically, the terpolymers of these formulations have a melt index of 0.5 to 200 and contain: l at least 65 percent, by weight, of ethylene, (2) at least 5 percent, by weight, of a second ethyleneically unsaturated monomer which is an ester of the group consisting of the vinyl esters of the lower (1-6 carbon) saturated aliphatic carboxylic acids, the alkyl acrylates, the alkyl methacrylates, the dialkyl maleates and the dialkyl fumarates of the lower l6 carbon) aliphatic alcohols; and (3) 0.01 to 3 percent, 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 alkyl hydrogen fumarates; the monoacrylates and monomethylacrylates of glycols', 2-hydroxy-3-aminopropyl allyl ether, allyl glycerol ether, divinyl glycol, Z-dimethylaminoethyl acrylate, Z-dimethylaminoethyl methacrylate and N-vinyl pyrrolidone. The preparation of the above-described terpolymer improving agents is more fully disclosed in U.S. Pat. No. 3,2l5,657, issued Nov. 2, 1965.
The thickening agents employed in the greases of the present invention comprise calcium complex soaps, including calcium acetate complex soaps and calcium lead acetate complex soaps.
Oils used in the greases of this invention can be min eral or synthetic oils of lubricating viscosity. Suitable mineral oils have a viscosity (SUS) of at least 40 seconds at 100F, and particularly those within the range of about 60 seconds to about 6,000 seconds at 100F.
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 pentacrythritol esters, di(2-ethyl hexyl) sebacate, di-(2-ethyl hexyl) adipate, dibutyl phthalate, polyethylene glycol di(2- atoms per molecule in the presence of an aliphatic halide and a Zielger-type catalyst.
With reference to the terpolymer improving agents of the present invention, preferred terpolymers contain from about 20 to about 30 percent, by weight, of the aforementioned group (2) component, i.e. the second ethylenically unsaturated monomer component; and from about 0.1 to about 1 percent, by weight, of the aforementioned group (3) component, i.e. the third ethylenically unsaturated monomer component. Representative preferred terpolymers comprise, in addition to ethylene, from about 20 to about 30 percent, by weight, vinyl acetate and from about 0.1 to about 1 percent, by weight, acrylic acid; from about 20 to about 30 percent, by weight, vinyl acetate and from about 0.1 to about l%, by weight, methacrylic acid; from about 20 to about 30 percent, by weight, ethyl acrylate and from about 0.1 to about 1 percent, by weight, acrylic acid; from about 20 to about 30 percent, by weight, ethyl acrylate and from about 0. l to about 1 percent, by weight methacrylic acid; from about 20 to about 30 percent by weight, methyl methacrylate, and from about 0.1 to about 1 percent, by weight, acrylic acid; and from about 20 to about 30 percent, by weight, methyl methacrylate and from about 0.l to about 1 percent, by weight, methacrylic acid.
Insofar as the quantity of terpolymer improving agent is concerned, the latter as previously indicated, is employed in a minor amount sufficient to incorporate in the grease formulation the desired resistance to Water wash-out 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 percent, by weight, and for most purposes, the presence of the terpolymer in an amount from about 0.] to about 5 percent, by weight, produces highly satisfactory improved grease compositions.
In preferred modifications, the terpolymer contains from about 20 to about 30 percent, by weight, of the group (2) monomer component and from about 0.1 to about 1 percent, by weight, of the group (3) monomer component. A particularly preferred terpolymer is one having a melt index of about 6 and containing about 71.8 percent, by weight, ethylene, about 25 percent, by weight, vinyl acetate and about 0.7 percent, by weight, methacrylic acid.
In accordance with the procedure set forth in the aforementioned U.S. Pat. No. 3,705,853, the abovedescribed greases are prepared by conventional grease manufacturing procedures which are well known to those skilled in the art. In such conventional procedures, it has heretofore been the practice to introduce the vehicle and thickening agent components into the mixing vessel or contactor. After saponification and an ultimate grease formulation has been achieved, in accordance with usual procedure, the aforementioned terpolymer is added to the finished grease to achieve the ultimate desired product. In following such procedure, however, it has been found that complete dispersion of the terpolymer is a calcium complex soap grease (including calcium acetate complex grease and calcium lead-acetate complex grease) is not achieved and, in many instances, a satisfactory yield is not obtained.
SUMMARY OF THE INVENTION In accordance with the present invention, it has now been found that a more complete dispersion of the aforementioned terpolymer, improved yields are ob tained and use of hiterto unsuitable oils are able to be incorporated in calcium complex greases by introducing the terpolymer in the charge of lubricating vehicle and thickening agent components prior to saponifi- 5 cation. Those skilled in the art have long recognized the influence of oils in various soap-base systems in that calcium acetate complex and calcium lead acetate complex grease bases are affected, for example, by substituting a paraffin oil for a naphthenic base oil. Naphthenic base oils notably result in a firm-bodied soap base, thereby resulting in good yield. Paraffin oils, on the other hand, in the same soap base, yield soft-bodied bases resulting in relatively poor yields.
DESCRIPTION OF SPECIFIC EMBODIMENTS In order to demonstrate the improvement realized in obtaining more complete dispersion of the aforementioned terpolymers, improvement in yield, and use of hitherto unsuitable oils are able to be incorporated in calcium complex greases by introducing the terpolymer to the charge of lubricating vehicle and thickening agent components prior to saponification, comparative data were obtained, as shown in the examles of the following Tables I and II. The grease-making technique employed in the examples ofTables I and II, in general, involves charging a contactor with appropriate amounts of fatty saponifable material, lime, litharge, water and base oil After saponification, the soap base is discharged to a finishing kettle. In some examples the terpolymer was added at this point, in other examples it constituted a part of the orginal charge to the contactor. In the former cases dehydration of the soap base is concurrent with dispersion of the terpolymer therein. Cooling, addition of various additive packages, homoginization and final addition of oil, complete the manufacture. The terpolymer employed in the examples of Tables I and II had a melt index of about 6 and contained about 71.8 percent, by weight, ethylene, about percent, by weight, vinyl acetate and about 0.71 percent, by weight, methacrylic acid. The base oils employed in the examples of Table I comprised either a 500 SUS solvent naphthenic neutral oil, with a V.l. of 60 or 300 SUS solvent paraffinic neutral oil having a VI. of 90. The base oils employed in the examples of Table II comprised either a 900 SUS solvent naphthenic neutral oil having a V.I. of 65 or a 300 SUS solvent paraffinic neutral oil having a \/.l. of 90.
INFLUENCE OF TERPOLYMER OF YIELD (Z FATTY MATERIAL) AND BASE OII. ON THE MANUFACTURE OF CALCIUM-LEAD ACETATE COMPLEX AND CALCIUM ACETATE COMPLEX GREASES TABLE I CALCIUM-LEAD ACETATE COMPLEX GREASES Ter- Fatty polymer Added Material Base Oil Consistency Ex. Present To '75 Type UW/W l I No W 12.0 Naphthenic 3 l9/328 2 Yes Finishing I21) Naphthenic 267/298 Kettle 3 Yes Contactor 10.5 Naphthcnic 280/301 Charge 4 No I50 Paraffinic 365/378 5 Yes Finishing I50 Paraffinic 347/36l Kettle 6 Yes Contactor l l.U Paraffinic 277/295 Charge INFLUENCE OF TERPOLYMER OF YIELD FATTY MATERIAL) AND BASE OIL ON THE MANUFACTURE OF CALCIUM-LEAD ACETATE COMPLEX AND CALCIUM ACETATE COMPLEX GREASES l J UW/W Unworked/btl Stroke Worked, ASTM D-2 l7 As will be apparent from the comparative examples of Tables I and II, significantly higher amounts of fatty material or softer consistency results are encountered in the finished grease where the terpolymer is either absent, (Examples I and 4 in each table), or introduced into the finished grease (Examples 2 and 5 in each table,) contrasted with the presence of significantly smaller amounts of fatty material or firmer consistency results when the terpolymer is introduced in the charge to the contactor (Examples 3 and 6 in each table).
While this invention has been described with reference to preferred compositions and components therefor, it will be understood by those skilled in the art that departure from the preferred embodiments can be effectively made and are within the scope of the specification.
I claim:
1. In a process for manufacturing a calcium complex grease in which there is incorporated an ethylene-vinyl ester-organic acid terpolymer as an improving agent, the method for improving grease formation which comprises introducing said terpolymer to the charge of lubricating vehicle and thickening agent components prior to saponification.
2. A process, as defined in claim 1, wherein the vehicle of said grease comprises a paraffinic mineral lubricating oil.
3. A process, as defined in claim I, wherein the vehicle of said grease comprises a synthetic lubricating oil.
4. A process, as defined in claim 1, wherin said terpolymer is present in said grease in an amount of at least 0.0l%, by weight.
5. A process, as defined in claim I, wherein said terpolymer is present in said grease in an amount from about 0.1 to about 5 percent, by weight.
6. A process, as defined in claim 1, wherein said grease composition comprises 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: l at least 65 percent, by weight, of ethylene, (2) at least 5 percent, 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 l6 carbons; the alkyl acrylatcs, the alkyl methacrylates, the dialkyl maleates and the dialkyl fumarates of aliphatic alchols having 1-6 carbons; and (3) 0.0l to 3 percent, 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 alkyl hydrogen fumarates', the monoacrylates and monomethyacrylates of glycols; 2-hydroxy-3- aminopropy] allyl ether, allyl glycerol ether, divinyl glycol, Z-dimethylaminomethyl acrylate, 2- dimethylaminoethyl methacrylate and N-vinyl pyrrolidone.
7. A process, as defined in claim 6, wherein said terpolymer contains from about to about percent, by weight of the group (2) monomer component.
8. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, of the group (2) component and from about 0.1 to about 1 percent, by weight, of the group (3) monomer component.
9. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, of vinyl acetate and from 0.1 to about 1 percent, by weight, acrylic acid.
10. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, vinyl acetate and from about U. l to about 1 percent, by weight, methacrylic acid.
11. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, ethylacrylate and from about 0.1 to about 1 percent, by weight, acrylic acid.
12. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, ethylacrylate and from about 0. l to about 1 percent, by weight, methacrylic acid.
13. A process, as defined in claim 1, wherein the terpolymer contains from about 20 to about 30 percent, by weight, methylmethacrylate and from about 0.1 to about 1 percent, by weight, acrylic acid.
14. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, methylmethacrylate and from about 0.1 to about 1 percent, by weight, mcthacrylic acid.
15. A process, as defined in claim 6, wherein the terpolymer has a melt index of about 6 and contains about 7.18 percent, by weight, ethylene, about 25.0 percent, by weight, vinyl acetate and about 0.7 percent, by
weight, methacrylic acid.
UNITED STATES PATENT AND TRADEMARK OFFICE CERTIFICATE OF CORRECTION PATENT NO. 3,904,534
DATED September 9, 1975 |NVENTOR(S) I FRANCIS S. SAYLES It is certified that error appears in the ab0ve-identified patent and that said Letters Patent are hereby corrected as shown below:
Column 6, line 22, "7.18" should read -7l.8-
Signed and Scaled this Attest:
RUTH C. MASON C. MARSHALL DANN Alresnng Officer Commissioner of Patents and Trademarks

Claims (15)

1. IN A PROCESS FOR MANUFACTURING A CALCIUM COMPLEX GREASE IN WHICH THERE IS INCORPORATED AN ETHYLENE-VINYL ESTER-ORGANIC ACID TERPOLYMER AS AN IMPROVING AGENT, THE METHOD FOR IMPROVING GREASE FORMATION WHICH COMPRISES INTRODUCING SAID TERPOLYMER TO THE CHARGE OF LUBRICATING VECHILE AND THICKENING AGENT COMPONENTS PRIOR TO SAPONIFICATION.
2. A process, as defined in claim 1, wherein the vehicle of said grease comprises a paraffinic mineral lubricating oil.
3. A process, as defined in claim 1, wherein the vehicle of said grease comprises a synthetic lubricating oil.
4. A process, as defined in claim 1, wherin said terpolymer is present in said grease in an amount of at least 0.01%, by weight.
5. A process, as defined in claim 1, wherein said terpolymer is present in said grease in an amount from about 0.1 to about 5 percent, by weight.
6. A process, as defined in claim 1, wherein said grease composition comprises 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 percent, by weight, of ethylene, (2) at least 5 percent, 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 alchols having 1-6 carbons; and (3) 0.01 to 3 percent, 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 alkyl hydrogen fumarates; the monoacrylates and monomethyacrylates of glycols; 2-hydroxy-3-aminopropyl allyl ether, allyl glycerol ether, divinyl glycol, 2-dimethylaminomethyl acrylate, 2-dimethylaminoethyl methacrylate and N-vinyl pyrrolidone.
7. A process, as defined in claim 6, wherein said terpolymer contains from about 20 to about 30 percent, by weight of the group (2) monomer component.
8. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, of the group (2) component and from about 0.1 to about 1 percent, by weight, of the group (3) monomer component.
9. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, of vinyl acetate and from 0.1 to about 1 percent, by weight, acrylic acid.
10. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, vinyl acetate and from about 0.1 to about 1 percent, by weight, methacrylic acid.
11. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, ethylacrylate and from about 0.1 to about 1 percent, by weight, acrylic acid.
12. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, ethylacrylate and from about 0.1 to about 1 percent, by weight, methacrylic acid.
13. A process, as defined in claim 1, wherein the terpolymer contains from about 20 to about 30 percent, by weight, methylmethacrylate and from about 0.1 to about 1 percent, by weight, acrylic acid.
14. A process, as defined in claim 6, wherein the terpolymer contains from about 20 to about 30 percent, by weight, methylmethacrylate and from about 0.1 to about 1 percent, by weight, methacrylic acid.
15. A process, as defined in claim 6, wherein the terpolymer has a melt index of about 6 and contains about 7.18 percent, by weight, ethylene, about 25.0 percent, by weight, vinyl acetate and about 0.7 percent, by weight, methacrylic acid.
US484909A 1974-07-01 1974-07-01 Grease manufacture Expired - Lifetime US3904534A (en)

Priority Applications (12)

Application Number Priority Date Filing Date Title
US484909A US3904534A (en) 1974-07-01 1974-07-01 Grease manufacture
ZA4010A ZA754010B (en) 1974-07-01 1975-06-23 Grease manufacture
GB26946/75A GB1507697A (en) 1974-07-01 1975-06-25 Paraffinic base greases
GB13087/76A GB1507698A (en) 1974-07-01 1975-06-25 Preparation of greases
DE2560382A DE2560382C2 (en) 1974-07-01 1975-06-26 Lubricating grease with a paraffinic mineral oil as a lubricant carrier
DE2528600A DE2528600C2 (en) 1974-07-01 1975-06-26 Process for the production of greases thickened with calcium or calcium-lead complex soaps and containing an organic terpolymer
US05/590,760 US3997455A (en) 1974-07-01 1975-06-26 Paraffinic base greases
CA230,533A CA1050524A (en) 1974-07-01 1975-06-30 Grease manufacture
AU82594/75A AU497712B2 (en) 1974-07-01 1975-06-30 Calcium complex grease
FR7520669A FR2277143A1 (en) 1974-07-01 1975-07-01 GREASES BASED ON PARAFFINIC OILS THICKNESS WITH A SOAP COMPLEX OF CALCIUM OR CALCIUM / LEAD
JP50080576A JPS5925836B2 (en) 1974-07-01 1975-07-01 Lubricating grease and its manufacturing method
JP55085270A JPS6019954B2 (en) 1974-07-01 1980-06-25 Lubricating grease manufacturing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US484909A US3904534A (en) 1974-07-01 1974-07-01 Grease manufacture

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US05/590,760 Continuation-In-Part US3997455A (en) 1974-07-01 1975-06-26 Paraffinic base greases

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US3904534A true US3904534A (en) 1975-09-09

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US (1) US3904534A (en)
JP (2) JPS5925836B2 (en)
AU (1) AU497712B2 (en)
CA (1) CA1050524A (en)
DE (2) DE2528600C2 (en)
FR (1) FR2277143A1 (en)
GB (2) GB1507697A (en)
ZA (1) ZA754010B (en)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
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

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6391538A (en) * 1986-10-06 1988-04-22 Kanebo Ltd Illumination apparatus

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3705853A (en) * 1970-09-23 1972-12-12 Mobil Oil Corp Grease compositions

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Publication number Priority date Publication date Assignee Title
US2833718A (en) * 1955-06-17 1958-05-06 Exxon Research Engineering Co Lubricating composition containing polyethylene resins
DE1258536B (en) * 1960-11-07 1968-01-11 Shell Res Ltd Process for producing a lubricating grease
BE786090A (en) * 1971-07-12 1973-01-10 Texaco Development Corp WATER-RESISTANT GREASE COMPOSITIONS
FR2205570B1 (en) * 1972-11-07 1976-06-04 Mobil Oil France

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3705853A (en) * 1970-09-23 1972-12-12 Mobil Oil Corp Grease compositions

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Also Published As

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CA1050524A (en) 1979-03-13
FR2277143B1 (en) 1981-08-07
GB1507698A (en) 1978-04-19
AU8259475A (en) 1977-01-06
DE2528600A1 (en) 1976-01-22
ZA754010B (en) 1977-01-26
JPS6019954B2 (en) 1985-05-18
FR2277143A1 (en) 1976-01-30
JPS5124604A (en) 1976-02-28
GB1507697A (en) 1978-04-19
AU497712B2 (en) 1979-01-04
JPS56127691A (en) 1981-10-06
DE2560382C2 (en) 1986-07-17
DE2528600C2 (en) 1982-12-23
JPS5925836B2 (en) 1984-06-21

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