US3384582A - Dispersions and greases - Google Patents

Dispersions and greases Download PDF

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Publication number
US3384582A
US3384582A US580868A US58086866A US3384582A US 3384582 A US3384582 A US 3384582A US 580868 A US580868 A US 580868A US 58086866 A US58086866 A US 58086866A US 3384582 A US3384582 A US 3384582A
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Prior art keywords
molybdenum disulphide
oleophilic
oil
dispersions
grinding
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US580868A
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Groszek Aleksander Jerzy
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BP PLC
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BP PLC
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • 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
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
    • 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

  • This invention relates to novel lubricating greases and to dispersions with improved lubricating properties.
  • a lubricating composition according to the invention is provided which is based on a mineral or synthetic lubrieating base oil and contains an oleophilic molybdenum disulphide, as hereinafter defined.
  • the oleophilic molybdenum disulphide used as the thickening agent in the dispersions or greases according to the invention is prepared by grinding natural or synthetic molybdenum disulphide in a low viscosity, low surface tension organic liquid.
  • molybdenum disulphide product prepared in this Way will hereinafter be called oleophilic molybdenum disulphide to distinguish it from the untreated starting material.
  • Oleophilic molybdenum disulphide has a considerable tendency to absorb ndotriacontane in preference to n-butanol in contrast to the untreated starting material.
  • Both natural and synthetic molybdenum disulphide are well-known and readily available.
  • One example of a natural molybdenum disulphide product is that supplied by Acheson Colloids, Dag 325.
  • Satisfactory products can be obtained by grinding in most organic liquids, but it is desirable to use one the bulk bulk of which can be easily removed from the oleophilic molybdenum disulphide. Those liquids distilling below 500 C. and having a viscosity below 600 centistokes at 100 F. (38 C.) are therefore preferred. Liquids having a surface tension below 72 degrees/cm, preferably from 10 to 40 degrees/cm, at 25 C. are preferred.
  • Suitable organic liquids are lower molecular weight hydrocarbons, including straight-chain or branched-chain, saturated or unsaturated alkyls, saturated or unsaturated, substituted or unsubstituted, cycloalkyls, and substituted or unsubstituted aromatic compounds. Examples of such compounds are n-heptane, octene-Z, 2,2,4-trimethylpentane, cyclohexane benzene or toluene. Branched alkyl compounds are particularly preferred.
  • Other suitable organic liquids are those compounds which contain fluorine, chlorine, or phosphorus and chlorine, for example, carbon tetrachloride.
  • Suitable organic liquids are the polar oxygen compounds such as isopropyl alcohol. Silicone fluids can also be used.
  • the amount of molybdenum disulphide in the molybdenum disulphide/organic liquid mixture should not exceed wt.; preferably it should be from 2 to 20% wt.
  • the grinding may be carred out in any suitable grinding mill or device and it is desirable to continue the grinding until an oleophilic molybdenum disulphide having a Patented May 21, 1958 ICC surface area (as determined by nitrogen adsorption) of from 10 to 400, preferably from 30 to 200, square metres per gram is obtained.
  • an oleophilic molybdenum disulphide having a Patented May 21, 1958 ICC surface area (as determined by nitrogen adsorption) of from 10 to 400, preferably from 30 to 200, square metres per gram is obtained.
  • this can be achieved by grinding at normal temperatures for the required period but the temperature of the mixture may be artificially increased if desired, for example, up to 400 C.
  • liquids which have viscosities up to 600 centistokes at F. (38 C.) may be used, for example, mineral lubricating oils, ranging from spindle oils to bright stocks.
  • One of the quickest and most effective techniques is to carry out the grinding in a vibratory ball mill.
  • Vibratory ball mills usually contain steel balls and these are suitable for the present purpose. It is preferred to use a hard grade of steel for the balls.
  • a magnetic filter can be used to remove small steel particles from the slurry.
  • a circulatory system can also be used wherein the slurry is pumped through an internal magnetic filter and then return to the mill.
  • a suitable vibratory ball mill is sold under the trade name Megapact, manufactured by Pilamec Limited.
  • the grinding effect is produced by the impact of the balls upon the molybdenum disulphide and upon each other.
  • the slurry of oleophilic molybdenum disulphide can be separated from the balls by sieving or by displacement by another liquid and sieving.
  • a relatively high boiling organic liquid is used for grinding it is preferred to displace this liquid by a low boiling liquid. This liquid can then be removed by boiling. It is preferred to use vigorous boiling.
  • the lubricating base oil may be a mineral oil or a synthetic oil.
  • Suitable mineral oils are refined mineral oils obtained from petroleum, for example, those having a viscosity at 210 F. within the range from 2 to 50 centistokes, preferably from 4 to 40 centistokes.
  • Synthetic lubricating oils include organic esters, polyglycol ethers, polyphenyl ethers, fluorinated hydrocarbons, silicate esters, silicone oils and mixtures thereof.
  • the most important class of synthetic oils are the organic liquid polyesters, particularly the neutral polyesters, having a viscosity at 210 F. within the range from 1 to 30 centistokes.
  • the expression polyester is used to mean esters having at least two ester linkages per molecule.
  • the expression neutral is used to mean a fully esterified product.
  • suitable polyesters include liquid diesters of aliphatic dicarboxylic acids and monohy-dric alcohols (for example, dioctyl sebacate, dinonyl sebacate, octyl nonyl sebacate, and the corresponding azelates and adipates), liquid diesters of aliphatic dicarboxylic acids and phenols (for example, those described in copending US. patent application Ser. No. 382,964, filed July 15, 1964, UK. patent application 19,687/63, US. patent application Ser. No. 400,243, filed Sept. 29, 1964, US. patent application Ser. No. 434,-
  • the amount of oleophilic molybdenum disulphide required to thicken the base oil will depend on the nature of the oil and the consistency of grease required. For most purposes an amount up to 50% wt., based on the final grease, will be used, generally 40% wt.
  • the oleophilic molybdenum disulphide can be incorporated into a grease by a numberof methods. It is preferred to incorporate the oleophilic molybdenum disulphide into a grease, immediately after grinding. However, if the oleophilic molybdenum disulphide is prepared some time before incorporation into the grease, it is preferred to store the oleophilic molybdenum disulphide in an airtight container to prevent deterioration.
  • the slurry of ground oleophilic molybdenum disulphide can be converted into a grease by, for example:
  • the grinding fluid is filtered oil".
  • the resulting filter cake is ground by, for example, feeding the cake through a colloid mill and stirring the resulting powder into the oil.
  • the resulting grease is finished by colloid milling.
  • Oil is added to the slurry of molybdenum disulphide and the mixture circulated through a homogeniser (for example, of the Manton-Gaulin type) so that temperatures up to or exceeding 140 C. are produced.
  • the temperature must be high enough to drive off the grinding fluid.
  • Molybdenum disulphide might also be ground directly in the base oil for the grease.
  • a low boiling point, low viscosity, low surface tension mineral lubricating oil with a viscosity up to 600 centistokes at 100 F. (38 C.) can be used. Elevated temperatures up to 400 C. can be used during the grinding.
  • oleophilic molybdenum disulphides can be incorporated into the base oil either at ambient temper-atures or, if desired, example, up to 400 C.
  • the greases according to the invention have remarkably high drop points. When their drop points are measused according to the IP or ASTM standard methods, they are found to be above 400 C.; such greases are described as infusible and are diffi'cult to produce by conventional methods.
  • base oils for example, synthetic oils with high oxidation and thermal stability, greases having a unique combination of properties can be produced.
  • improv ers metal deactivators, anti-corrosion agents, antioxidants etc. can also be added to the greases.
  • Loadcarrying additives can also be added to the greases according to the invention.
  • the greases according to the invention have been found to be infusible, that is, they show no dropping point at temperatures up to 400 C. (using either the IP 31 test or the ASTM Method D566-42).
  • the combination of temperature-stable synthetic base oils, for example, the polyphenyl others, with oleophilic molybdenum disulphide has been found to show remarkable high temperature DISPERSIONS Oleophilic molybdenum disulphide can be incorporated into base oils in quantities up to 30% wt., based on the total wt., generally 130%, to form dispersions with surprisingly good lubricating properties.
  • the dispersions are remarkably stable even without the dispersants usually employed to stabilise the dispersion.
  • surface active agents etc. can in some cases be added to the oleophilic molybdenum disulphide either during or after grinding and the ease of dispersion of the oleophilic molybdenum disulphides might, thereby, be increased
  • the dispersions can be formed quite simply by stirring the oleophilic molybdenum disulphide into the base oil.
  • a mechanical aid to dispersion such as a colloid mill can be used.
  • the base oils used for the dispersion are the same as those used for grease and described above. Usually 2 to 20% wt. M08 will be used.
  • the properties of lubricating dispersions can conveniently be evaluated in the well-known Four Ball EP Lubricant Test Machine. The method of test isas prescribed in US. Federal Test Method Standard No. 791a Method 6503.1.
  • the load-carrying properties of the dispersions according to the invention are conveniently evaluated by measuring the wear scar diameters on the balls of this ma chine when lubricated by the dispersions under various loads and after known time intervals.
  • the load-carrying properties of the dispersions according to the invention are found to be considerably superior to those of suspensions of air-ground molybdenum disulphide.
  • Dispersions of molybdenum disulphides which have been ground in solvents such as fiorinated or chlorinated hydrocarbons, or solutions of chlorinated hydrocarbons, or sulphur-containing or phosphorus-containing compounds in hydrocarbons, for example, carbon tetrachloride, have improved load-carrying properties.
  • EXAMPLE 1 The properties of two greases according to the invention prepared using oleophilic molybdenum disulphide are molybdenum disulphide may .be aided. Viscosity index given in Table I below.
  • B G 150[75 refers to a basic grade mineral oil having a Redwood I Viscosity of 150 seconds (36.4 centrstokes) at F. (60 0.) and a viscosity index of 75.
  • Grease A was prepared by stirring the oleophilic molybdenum disulphide into the base oil at room temperature, followed by passing the mixture through a colloid mill.
  • Grease B was prepared by adding the oils to the slurry of molybdenum disulphide in n-heptane and distilling off the latter.
  • Base oil plus 5% M08 commercial, A (fine) 0. 40 0.77 1. 44 2. 29 3. 07/3. 6
  • Base oil plus M032 commercial, A (fine) 0.39 0.74 1. 66 1. 71 2. 57/2. 63
  • Base oil plus 10% M082 commercial, A (very fine)- 0. 41 0. 69 1. 84 1. 79 2. 60/2.
  • Base oil plus 2% MOSz commercial, 0 0. 45 0. 73 1. 22 1. 83 2.46/2.
  • Base oil plus 4% M082 commercial, 0.. 0. 45 0. 73 0.82 2. 09 2. 53/2. 13 Do 0. 39 0.71 0. 84 1.74 2. 33/2. 5
  • Base oil plus 5% oleophilic MOSz (average of 3 results) 0. 41 0. 60 0. 00 2. 3/2. 4
  • the base oil was a mineral lubricating oil, Redwood I viscosity at 140 F. (60 C.) of100 seconds and a VI 2 I he oleophilic MOS: was ground in -heptane for 8 hours.
  • Base o il (Medicinal paraffin oil) 18 Mediclnal parafiin oil plus 5% oleophilic 1 Ground for 8 hours in n-heptane.
  • a lubricating composition which is based on a lubricating base oil and containing an elfective amount of an oleophilic molybdenum disulphide having a surface area of 10 to 400 square metres per gram and prepared by grinding natural or synthetic molybdenum disulphide in an organic liquid distilling below 500 (3., having a viscosity below 600 centistokes at 38 C. and having a surface tension below 72 degrees/ cm. at 25 C.
  • a lubricating composition as claimed in claim 1 which comprises up to 50% by weight of oleophilic molybdenum disulphide, based on the total weight of composition.
  • a method of preparing a lubricating composition comprising forming a mixture which consists of less than 50% by weight of natural or synthetic molybdenum disulphide and an organic liquid distilling below 500 C., having a viscosity below 600 centistokes at 38 C. and having a surface tension below 72 degrees/cm.
  • a method of preparing a lubricating composition comprising forming a mixture which consists of less than 50% by weight of natural or synthetic molybdenum disulphide and a lubricating base oil distilling below 500 C., having a viscosity below 600 centistokes at 38 C. and having a surface tension below 72 degrees/cm. at 25 C., and grinding the molybdenum disulphide in the lubricating base oil until the molybdenum disulphide becomes oleophilic and has a surface area of 10-400 square meters per gram.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
US580868A 1965-09-24 1966-09-21 Dispersions and greases Expired - Lifetime US3384582A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB40699/65A GB1162222A (en) 1965-09-24 1965-09-24 Improved Dispersions and Greases

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US3384582A true US3384582A (en) 1968-05-21

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US (1) US3384582A (sl)
BE (1) BE687312A (sl)
DE (1) DE1594362A1 (sl)
GB (1) GB1162222A (sl)
NL (1) NL6613470A (sl)
SE (1) SE338633B (sl)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3518187A (en) * 1967-03-20 1970-06-30 British Petroleum Co Oleophilic tin sulphide
US5320761A (en) * 1991-02-22 1994-06-14 Pennzoil Products Company Lubricant fluid composition and methods for reducing frictional losses therewith in internal combustion engines
US20040092408A1 (en) * 2002-10-31 2004-05-13 Tomlin Scientific, Inc. Rock bit grease composition
US20050133265A1 (en) * 2003-12-23 2005-06-23 Denton Robert M. Rock bit with grease composition utilizing polarized graphite
US20060254823A1 (en) * 2005-05-16 2006-11-16 Smith International, Inc. Drill bit lubricant with enhanced load carrying/anti wear properties
US20070107940A1 (en) * 2005-11-14 2007-05-17 Smith International, Inc. Drill bit lubricant utilizing a sulfur-phosphorous EP agent
US20070254817A1 (en) * 2006-05-01 2007-11-01 Smith International, Inc. High performance rock bit grease

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3059769A (en) * 1959-04-14 1962-10-23 Cefilac Extrusion lubrication
US3338822A (en) * 1964-09-25 1967-08-29 British Petroleum Co Preferential adsorption of normal paraffins on molybdenum disulphide, tungsten disulphide and boron nitride

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3059769A (en) * 1959-04-14 1962-10-23 Cefilac Extrusion lubrication
US3338822A (en) * 1964-09-25 1967-08-29 British Petroleum Co Preferential adsorption of normal paraffins on molybdenum disulphide, tungsten disulphide and boron nitride

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3518187A (en) * 1967-03-20 1970-06-30 British Petroleum Co Oleophilic tin sulphide
US5320761A (en) * 1991-02-22 1994-06-14 Pennzoil Products Company Lubricant fluid composition and methods for reducing frictional losses therewith in internal combustion engines
US20040092408A1 (en) * 2002-10-31 2004-05-13 Tomlin Scientific, Inc. Rock bit grease composition
US7312185B2 (en) 2002-10-31 2007-12-25 Tomlin Scientific Inc. Rock bit grease composition
US20050133265A1 (en) * 2003-12-23 2005-06-23 Denton Robert M. Rock bit with grease composition utilizing polarized graphite
US7121365B2 (en) 2003-12-23 2006-10-17 Smith International, Inc. Rock bit with grease composition utilizing polarized graphite
US20060254823A1 (en) * 2005-05-16 2006-11-16 Smith International, Inc. Drill bit lubricant with enhanced load carrying/anti wear properties
US7267183B2 (en) 2005-05-16 2007-09-11 Smith International, Inc. Drill bit lubricant with enhanced load carrying/anti wear properties
US20070107940A1 (en) * 2005-11-14 2007-05-17 Smith International, Inc. Drill bit lubricant utilizing a sulfur-phosphorous EP agent
US20070254817A1 (en) * 2006-05-01 2007-11-01 Smith International, Inc. High performance rock bit grease
US7749947B2 (en) 2006-05-01 2010-07-06 Smith International, Inc. High performance rock bit grease

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Publication number Publication date
GB1162222A (en) 1969-08-20
BE687312A (sl) 1967-03-23
DE1594362A1 (de) 1970-10-22
SE338633B (sl) 1971-09-13
NL6613470A (sl) 1967-03-28

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