US2825694A - Process for the preparation of high temperature anti-friction bearing lubricants - Google Patents

Process for the preparation of high temperature anti-friction bearing lubricants Download PDF

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US2825694A
US2825694A US278432A US27843252A US2825694A US 2825694 A US2825694 A US 2825694A US 278432 A US278432 A US 278432A US 27843252 A US27843252 A US 27843252A US 2825694 A US2825694 A US 2825694A
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grease
soap
oil
mixture
mineral oil
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US278432A
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Arnold J Morway
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ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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Priority to BE518532D priority Critical patent/BE518532A/xx
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Priority to US278432A priority patent/US2825694A/en
Priority to GB2011/53A priority patent/GB745145A/en
Priority to DEST6156A priority patent/DE945174C/de
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    • C10M2229/043—Siloxanes with specific structure containing carbon-to-carbon double bonds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/044—Siloxanes with specific structure containing silicon-to-hydrogen bonds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • 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
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • 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 lubricating grease compositions and particularly to a method for the preparation of lubricating greases. More particularly the invention relates to a novel process for the preparation of lubricating grease compositions which utilizes a technique involving the application of shearing forces without concurrent mixing to obtain maximum soap dispersion.
  • the thixotropic nature of the soap thickener can be controlled to a greater extent and, in addition, the penetration of the final product can be easily adjusted to the desired level, i. e., a grease of a desired degree of hardness can be obtained.
  • the gist of the instant invention lies in the technique of'applying the shearing forces upon the grease crystals. This application of shearing must occur in the absence of any concurrent or simultaneous mixing. It is postulated that the action of shear, which, by definition, involves the application of force in a plane, disperses the soap in an intimately orientated linear pattern. In addition to this linear orientation, the small bundles or fibriles of soap crystals are sheared in a plane and the resulting dispersion approaches the ultimate. If the grease formulation is not subjected to mixing which is concurrent or simultaneous, the resulting dispersion is maintained. If, however, the application of shearing force is accompanied by a simultaneous or concurrent mixing eliect the soap crystals are congregated, the orientation disappears and the resulting dispersion pattern is the one with which the art is familiar.
  • Rates of shear varying from about 10,000 reciprocal seconds to 500,000 or more reciprocal seconds are pre- ICC ferred in practicing the process of this invention. As will be shown later, desirable consistency increase may be obtained with a rate of shear of about 10,000 or more, and the consistency of the grease formulation may be closely controlled by controlling the rate of shear in this range. Practical application for commercial use will ordinarily dictate the use of rates of shear within the range of 100,000 to 400,000.
  • the grease formulation is prepared by techniques which are familiar to the art.
  • the formulation is then subjected to a shearing force without concurrent or simultaneous mixing by causing the grease to flow at high velocity and high pressure under streamlined conditions.
  • These conditions may be obtained be equipment such as the Gaulin homogenizer, manufactured and sold by the Manton-Gaulin Manufacturing Company of Everett Massachusetts.
  • Rolling mills wherein the grease formulation passes through steel rollers with minute clearances, may be used.
  • the well known Morehouse Mill wherein the milled material passes through spinning dies at low clearances is operable.
  • a pressure viscosimeter if operated at sufiiciently high pressures may also be used.
  • Various other mechanical means may also. be used for the application of this shearing force, so long as there is present no concurrent mixing.
  • the process of the instant invention is applicable to grease compositions wherein the thickening agent is of a complex structure, that is to say, those greases which utilize as a thickening agent, or soap, a complex of two or more components may be prepared using the novel technique of the instant invention.
  • Such complex soap greases as those prepared using rapeseed oil soaps, those greases thickened with a complex of a high molecular weight soap and a low molecular weight salt such as ace tates, furoates, acrylates, etc. are'prepared using the process of this invention. So far as is known straight fatty acidsoap greas es may not be prepared by the technique outlined above.
  • the instant invention is particularly applicable for the preparation of anti-friction bearing lubricants.
  • the grease composition necessary to furnish the desired long and continuous lubrication at elevated temperature is a channeling type grease. That is to say, a grease which gives a low torque and low bearing temperature rise is needed since in an operating bearing of this type the grease is pushed out of the path of the rolling elements during the first few revolutions of the bearing. Thus no unnecessary power loss or heat buildup occurs in moving the grease in the bearing.
  • This immediate channeling type grease is obtained in the prior art by high soap concentration, the grease structure beingmodified during manufacture to obtain a relatively high penetration. This grease then acts as a lubricant reservoir and as a seal to prevent entrance of dirt and other undesirable contaminants into the lubricated bearing.
  • Desired amounts of refined, unblown, rapeseed oil and an equal to a'double portion of the desired mineral oil, along with a small amount of the sodium salt of a pctroleum sulfonate are charged to a fire-heated grease kettle.
  • the kettle is equipped with an eflicient agitator or mixing blades.
  • An amount of an aqueous caustic soda solution suflicient to give an excess of 0.3 to-0.6% sodium hydroxide, based on the finished grease, is then charged to the kettle.
  • the mass is heated to about 250 F. until saponification is completed and the soap is dehydrated.
  • the balance of the oil is then charged and the mass slowly heated to about 500 F., at which temperature it is completely molten.
  • the mixture is then cooled to 200 F. with stirring; The recrystallization of the soap occurs during this cooling period and inhibitors are added then.
  • the blend. product was soft and fluid having no meaningful penetration. subjected to various rates of shearing in a pressure viscosimeter. In this apparatus the grease was forced through a capillary 0.4 mm. in diameter and 16 mm.
  • the flow. rate was determined by collecting the outflowing grease The rate of shear in reciprocal seconds was calculated from the standard variation 0 v for a measured time.
  • Part B.A lubricating grease composition containing approximately 18.7% of the sodium soap of raw rapeseed oil was prepared in accordance with the process of the instant invention, that is to say, a base grease was prepared containing approximately 30% soap. It was then cooled to below the transition temperature of the soap (below about 200 F.). Sufficient mineral oil was added to result in the mass containing about 18.7% soap, based on the total product. Portion A was not homogenized, but portion B was passed through a Gaulin homogenizer at a discharge pressure of about 3,000
  • Part C.Another grease composition prepared in accordance with the process of instant invention contained approximately 12% of the sodium soap of rapeseed oil. Portion A was unhomogenized and portion B was homogenized. The samples were also submitted to the inspection tests as recorded in part A above. The inspection data on the grease samples are set out in Table II below: H
  • the resulting grease composition was subjected to v shearing'forces in the absence of concurrent mixing in a G'aulinhomogenizer at varying pressures.
  • the eflect of this treatment is set out in Table III below.
  • Part 1 A sample of this grease composition was submitted to a Gaulin homogenizer at various pressures.
  • complex soap structure of the furfural type greases may also be prepared by'the process of the instant invention.
  • this invention relates to an improved process for the preparation of lubricating grease compositions which utilizes a technique involving the application of shearing forces Without concurrent mix-' ing.
  • the process may 'be applied to control the con sistency of a finished grease composition using a lesser amount of soap than was hitherto thought possible.
  • a method for the preparation of lubricating grease compositions which COlIlPl'liES preparing a mixture of a complex soap and a mineral oil and hardening the mixture to the desired consistency by the application of shearing forces within a range of from 10,000 to 500,000 reciprocal seconds under streamlined conditions.
  • a method for controlling the consi tency of lubricating grease compositions having a complex soap structure which comprises subjecting the composition to the action of rates of shear within the range rorn 10,000 to 500,000 reciprocal seconds under streamlined conditions.
  • a method according to claim 2 wherein the complex soap is a rapeseed oil soap.
  • a method according to claim 2 wherein the complex soap is a complex of a high molecular weight soap and a low molecular weight salt.
  • a method for dispersion of complex soap crystals in a lubricating oil composition to form a grease composition of a controlled consistency which comprises subjecting a mixture of soap and oil to the action of shearing forces within the range of from 100,000 to 400,000 reciprocal seconds under streamlined conditions.
  • said complex soap is a complex of a high molecular weight soap and a low molecular weight salt.
  • a method for the preparation of lubricating grease compositions having ASTM penetration values within the range of 200 to 350 mm./ 10 which comprises forming a complex soap grease having from to 50% soap, adding additional lubricating oil to reduce the overall soap content to one within the range of from 6% to 18% soap, and subjecting the mixture to the action of shearing forces in the range of from 100,000 to 400,000 reciprocal seconds under streamlined conditions.
  • a method according to claim 10 wherein said complex soap is a rapeseed oil soap.
  • a method according to claim 10 wherein said complex soap is a complex of a high molecular weight soap and a low molecular weight salt.
  • a method according to claim 10 wherein said complex soap is prepared by subjecting furfural to the Cannizzaro reaction.
  • a method for the preparation of channeling type high temperature anti-friction bearing lubricating grease compositions which comprises saponifying rapeseed oil with caustic soda in the presence of a hydrocarbon by heating in the presence of free alkali to dehydrate the material, adding additional mineral oil while stirring, heating to a temperature between about 480 F. and 520 F., cooling the mixture to a temperature below the transition temperature of the soap, adding to the cooled mixture additional mineral oil to substantially reduce the soap content of the mixture and subjecting the total mixture to shearing action under streamlined conditions to obtain the final product.
  • a method for the preparation of channeling type high temperature anti-friction bearing lubricating grease composition containing from about 10% to about 15% soap which comprises saponifying raw rapeseed oil with caustic soda in the presence of a hydrocarbon oil by heating in the presence of free alkali to dehydrate the material, adding additional mineral oil while stirring, heating to a temperature or about 480 F. to 520 F., cooling the mixture to obtain a composition containing approximately 20% to 30% soap, adding to the cooled mixture additional mineral oil and subjecting the total mixture to an action of shearing forces in the range of from about 100,000 to about 500,000 reciprocal seconds under conditions of streamlined flow to obtain a final product.
  • the method of preparation of channeling type high temperature anti-friction bearing grease lubricating composition which comprises heating a mixture of mineral oil, a small amount of an oil-soluble sodium sulfonatc and sufficient rapeseed oil to give a final product containing 20% to 30% soap, adding aqueous sodium hydroxide in a slight excess over that necessary to completely saponity the rapeseed oil, further heating the rapeseed oil to dehydrate the mixture, adding additional mineral oil and continuing the heating to about 480 F. to 520 F.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
US278432A 1952-03-25 1952-03-25 Process for the preparation of high temperature anti-friction bearing lubricants Expired - Lifetime US2825694A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BE518532D BE518532A (xx) 1952-03-25
US278432A US2825694A (en) 1952-03-25 1952-03-25 Process for the preparation of high temperature anti-friction bearing lubricants
GB2011/53A GB745145A (en) 1952-03-25 1953-01-23 Improvements in or relating to lubricating grease compositions
DEST6156A DE945174C (de) 1952-03-25 1953-03-25 Verfahren zur Herstellung von Schmierfetten

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US278432A US2825694A (en) 1952-03-25 1952-03-25 Process for the preparation of high temperature anti-friction bearing lubricants

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US2825694A true US2825694A (en) 1958-03-04

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BE (1) BE518532A (xx)
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE547164A (xx) * 1955-04-22
JPH10130682A (ja) * 1996-10-29 1998-05-19 Ntn Corp グリース封入転がり軸受

Citations (21)

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GB190218249A (en) * 1902-08-19 1902-12-11 Auguste Gaulin Improved Process and Apparatus for Intimately Mixing Milk and other Fluids.
GB190322875A (en) * 1902-11-15 1903-11-26 Auguste Gaulin Improved Process and Apparatus for Intimately Mixing Milk and other Fluids.
GB190522941A (en) * 1905-02-03 1906-05-10 Auguste Gaulin Improvement in or relating to Apparatus for Fixing Milk.
US2108672A (en) * 1935-05-31 1938-02-15 Texas Co Grease manufacture
US2265791A (en) * 1939-04-06 1941-12-09 Standard Oil Dev Co Grease composition and method for making same
US2318668A (en) * 1940-06-24 1943-05-11 Standard Oil Dev Co Grease manufacture
US2383906A (en) * 1942-10-28 1945-08-28 Standard Oil Dev Co Improved manufacture
US2431453A (en) * 1944-12-30 1947-11-25 Standard Oil Dev Co Lubricant manufacture
US2433636A (en) * 1942-02-20 1947-12-30 Benjamin Clayton Manufacture of greases
US2459483A (en) * 1944-12-06 1949-01-18 Standard Oil Dev Co Continuous method for determining the apparent viscosity of a grease
US2461276A (en) * 1946-11-12 1949-02-08 California Research Corp Manufacture of soap-thickened compositions and apparatus therefor
US2478917A (en) * 1946-09-24 1949-08-16 George M Hain Method and apparatus for making grease
US2503676A (en) * 1948-10-11 1950-04-11 Gulf Research Development Co Viscometer
US2516137A (en) * 1948-10-30 1950-07-25 Standard Oil Dev Co High-temperature lubricating greases
US2542159A (en) * 1946-12-14 1951-02-20 Pure Oil Co Continuous grease manufacture
US2588556A (en) * 1949-05-16 1952-03-11 Shell Dev Manufacture of grease compositions
US2599343A (en) * 1950-02-08 1952-06-03 Standard Oil Dev Co High-temperature lubricating grease manufacture
US2610947A (en) * 1950-06-24 1952-09-16 Standard Oil Dev Co Lubricating grease and process of manufacture
US2626241A (en) * 1949-12-24 1953-01-20 Standard Oil Dev Co Bentonite greases
US2704363A (en) * 1954-06-14 1955-03-15 Socony Vacuum Oil Co Inc Grease manufacture
US2713790A (en) * 1951-10-12 1955-07-26 Texas Co Rotational viscometer

Patent Citations (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB190218249A (en) * 1902-08-19 1902-12-11 Auguste Gaulin Improved Process and Apparatus for Intimately Mixing Milk and other Fluids.
GB190322875A (en) * 1902-11-15 1903-11-26 Auguste Gaulin Improved Process and Apparatus for Intimately Mixing Milk and other Fluids.
GB190522941A (en) * 1905-02-03 1906-05-10 Auguste Gaulin Improvement in or relating to Apparatus for Fixing Milk.
US2108672A (en) * 1935-05-31 1938-02-15 Texas Co Grease manufacture
US2265791A (en) * 1939-04-06 1941-12-09 Standard Oil Dev Co Grease composition and method for making same
US2318668A (en) * 1940-06-24 1943-05-11 Standard Oil Dev Co Grease manufacture
US2433636A (en) * 1942-02-20 1947-12-30 Benjamin Clayton Manufacture of greases
US2383906A (en) * 1942-10-28 1945-08-28 Standard Oil Dev Co Improved manufacture
US2459483A (en) * 1944-12-06 1949-01-18 Standard Oil Dev Co Continuous method for determining the apparent viscosity of a grease
US2431453A (en) * 1944-12-30 1947-11-25 Standard Oil Dev Co Lubricant manufacture
US2478917A (en) * 1946-09-24 1949-08-16 George M Hain Method and apparatus for making grease
US2461276A (en) * 1946-11-12 1949-02-08 California Research Corp Manufacture of soap-thickened compositions and apparatus therefor
US2542159A (en) * 1946-12-14 1951-02-20 Pure Oil Co Continuous grease manufacture
US2503676A (en) * 1948-10-11 1950-04-11 Gulf Research Development Co Viscometer
US2516137A (en) * 1948-10-30 1950-07-25 Standard Oil Dev Co High-temperature lubricating greases
US2588556A (en) * 1949-05-16 1952-03-11 Shell Dev Manufacture of grease compositions
US2626241A (en) * 1949-12-24 1953-01-20 Standard Oil Dev Co Bentonite greases
US2599343A (en) * 1950-02-08 1952-06-03 Standard Oil Dev Co High-temperature lubricating grease manufacture
US2610947A (en) * 1950-06-24 1952-09-16 Standard Oil Dev Co Lubricating grease and process of manufacture
US2713790A (en) * 1951-10-12 1955-07-26 Texas Co Rotational viscometer
US2704363A (en) * 1954-06-14 1955-03-15 Socony Vacuum Oil Co Inc Grease manufacture

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GB745145A (en) 1956-02-22
DE945174C (de) 1956-07-05
BE518532A (xx)

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