US3108965A - Grease manufacture - Google Patents

Grease manufacture Download PDF

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Publication number
US3108965A
US3108965A US51139A US5113960A US3108965A US 3108965 A US3108965 A US 3108965A US 51139 A US51139 A US 51139A US 5113960 A US5113960 A US 5113960A US 3108965 A US3108965 A US 3108965A
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Prior art keywords
grease
soap
temperature
oil
mixture
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US51139A
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English (en)
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Richard A Butcosk
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ExxonMobil Oil Corp
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Socony Mobil Oil Co Inc
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Priority to NL268340D priority Critical patent/NL268340A/xx
Application filed by Socony Mobil Oil Co Inc filed Critical Socony Mobil Oil Co Inc
Priority to US51139A priority patent/US3108965A/en
Priority to GB28138/61A priority patent/GB993061A/en
Priority to FR871350A priority patent/FR1302054A/fr
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    • 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
    • C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • C—CHEMISTRY; METALLURGY
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/063—Peroxides
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C—CHEMISTRY; METALLURGY
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/024—Propene
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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    • C10M2207/24—Epoxidised acids; Ester derivatives thereof
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    • C10M2207/28—Esters
    • C10M2207/34—Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/105—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/109—Polyethers, i.e. containing di- or higher polyoxyalkylene groups esterified
    • C—CHEMISTRY; METALLURGY
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    • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/02—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/04—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen, halogen, and oxygen
    • C10M2211/042—Alcohols; Ethers; Aldehydes; Ketones
    • C—CHEMISTRY; METALLURGY
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    • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/06—Perfluorinated compounds
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C—CHEMISTRY; METALLURGY
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    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/042—Metal salts thereof
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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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    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
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    • C10N2010/00—Metal present as such or in compounds
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    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08—Resistance to extreme temperature
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/12—Gas-turbines
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy
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    • C10N2070/02—Concentrating of additives

Definitions

  • solution temperature is that temperature at which substantially complete solution of a soap thickening agent in the liquid lubricant occurs.
  • temperature at which the Tyndall beam disappears in the mixture is that temperature at which the Tyndall beam disappears in the mixture.
  • each grease is characterized by a solution temperature, it is also often characterized by one or more transition temperatures. That is, a soap can exist in different crystalline structures while the soap is in the solid state, insoluble in the oil portion. These crystalline structures differ in degree of crystalline order and degree of interpenetration of oleaginous vehicle with the soap crystalline structure. Each crystalline soap structure is stable over a definite but limited temperature range. Thus, the temperature at which a change occurs in the crystalline structure of the soap portion of a grease, is a transition temperature. It may also be regarded as a temperature at which a phase change occurs in the grease. Such a temperature is less than the already defined solution temperature.
  • the new process comprises: wetting a preformed soap with a vehicle at a temperature between about 25 0 F. and the decomposition temperature of either of the soap or vehicle, whichever is lower; subjecting the resulting soap-vehicle mixture at a temperature within the aforesaid range to mechanical atomization under a pressure of at least about 1000 p.s.i. and preferably at least about 2G00 p.s.i., to form dispersed droplets; and instantaneously contacting the droplets directly with a substantially cooler surrounding atmosphere to effect heat exchange.
  • the product so formed is a grease.
  • grease denotes a composition comprising a major proportion of an oil of lubricating Viscosity thickened to a grease consistency with a soap or soaps, the composition having an unworked penetration, when tested by ASTM Method D217-52T, of at most 475, using the modified cone recommended by ASTM Technical Committee G, of ASTM Committee D-2.
  • the primary object of the present invention is to provide a method for readily preparing a grease from a preformed soap or soaps.
  • Another object is to provide a continuous process in which products of uniform characteristics can be obtained.
  • FIGURE. 1 is ia highly-diagrammatic form of a typical system for practicing the invention.
  • FTGURE 2 shows a cross-section of a high pressure atomizing nozzle suitable for use herein.
  • Line 11 is a charge line for introducing soap and oil to contactor 10.
  • Line 12 carries pre-formed soap from storage 13 and connects with line 11.
  • line 14 carries oil from storage 15 and connects with line 11.
  • Heat is supplied to 10 -by circulating ho-t oil, steam or the like through line 16 and the jacket 17 thereof.
  • the pre-formed soap and oil are heated, to a temperature and for a time sufcient fto ensure wetting of soap with oil.
  • This temperature will be above about 250 F. and below the decomposition temperature of the soap or oil, whichever is lower.
  • Line 18 is provided at the top of contacter 1i), to serve as a vent, should it be desired to control pressure in lche contacter or to allow any volatile material in the charge to escape.
  • air or other gas can be introduced into line 19 under pressure to convey the heated mixture though line Ztl and valve Z1 to spray manifold 22, lines 23 and nozzle 24.
  • the gas pressure should be at least sufficient for the atomization required in nozzles 2,4%; that is, the pressure should be at least about 1000' p.s.i.
  • Spray manifold 2v2 can comprise a 2 inch pipe having four 1/2 inch pipes Z2.
  • Each of lines 22 is equipped Iwith an Iatomizing noznle 24.
  • the mixture in lines 23 is a mixture of soap wetted with oil.
  • the mixture does not have the consistency of a grease, nor does the soap separate from the oil.
  • mixture Iin lines 23 passes through nozzles 24 into receiver 26 such as a grease kettle equipped with either or both of a motor-driven, multi-bladed agitator 27 and a motor-driven, paddle-type agitator 28.
  • receiver 26 such as a grease kettle equipped with either or both of a motor-driven, multi-bladed agitator 27 and a motor-driven, paddle-type agitator 28.
  • These agitators serve to eiect removal of product from the walls and bottom ⁇ of kettle 26.
  • the temperature of product in 26 can be regulated by oil, steam or the like circulating through line 29 and jacket 30. Finely dispersed droplets are discharged from nozzles y24tinto receiver 26 and are contacted with a surrounding atmosphere in receiver 26. As the product emerges from nozzles 24, it is cooled substantially by the surrounding atmosphere.
  • Air can be admitted to receiver '26 through inlets 31 surrounding lines 23, to regulate the amount of cooling desired of the product dischanged from nozzles 24.
  • atmospheres otherthan air can be used and that such can be introduced through inlets 31.
  • nitrogen, carbon dioxide, flue gas, steam and the like can be used.
  • Grease in receiver 26 is removed through valved line 34 by pump 35 and is discharged into valved line 36. lf desired, the product can be recycled through valved line 37 for return to receiver 26. This is advantageous to aid in mixing vehicle or additive charged through valved line 38 with product collected in receiver 26.
  • the product in line 35 can also be recycled through lines 37 and 39 to nozzles 24 by way of 21, 22 and 23. This is advantageous in the event further atomizaton of the grease product should be desired.
  • the grease product in receiver is generally highly aerated. lt is removed through valved line 34 by pump 35 and is passed through line 36 to deaeration in deaerator 40.
  • the latter can be any of those usual in the art, such Ias a Morehouse Deaerator, a Connell Cold Grease Homogenizer, a Kinney Heli-Quad vacuum pump, or of the type described by Brooke and Piazza in U.S. Patent No. 2,797,767. These devices igenerally operate on a vacuum principle.
  • Grease emergent from deaerator 40 through line 41 can be pumped by pump 42 and line 43 through a conventional lter 44.
  • the ⁇ finished grease is taken through line 4S and is packaged in equipment designated 46.
  • Line 47 in line 20, is provided as a pressure ⁇ release line for safety purposes.
  • FIGURE 2 reveals, in cross-section, a typical high pressure atomizing nozzle :found etective for the mechanical atomization of this invention.
  • Ilh-is is composed of body 50 containing ow path 51.
  • the core is held in place by orifice cap 54 which is secured to body 50 as shown.
  • FIGURE 2 This causes the stream of material to exit from orifice 56 as a hollow cone which atomizes into a hollowi cone spray.
  • This fitting of FIGURE 2 is oi heavy construction, being designed for pressures in passage 55 of at least 1000 p.s.i. and preferably up to several thousands of pounds per square inch.
  • Such a nozzle is supplied by Spraying Systems Company, and is identified as 1/2 SB 30 Nozzle, Number 40 Core.
  • su-ch devices in place of the atomizing ⁇ device illustrated by FIG- URE 2, other su-ch devices known in the art can be used so long as the operating pressure is at least about 1000 p.s.i.
  • the following can be mentioned: impinging jet nozzles, centrifugal or rotating disc atomizers,
  • pneumatic aftomizers pneumatic aftomizers, vibrating atomizers, multi-jet atom-A izers, impact type nozzles and other liquid dispensing devices.
  • EXAMPLE l This involves the preparation of a grease of the character defined in U.S. Patent No. 2,842,494.
  • the grease is comprised of lithium stearate (8 percent by weight), lithium soaps of wool grease fatty acids (3 percent by weight), dipropy'lene -glycol pelangonate (66.5 percent by weight) and a naphthenic mineral oil, 750 seconds S.U.S. at 100 F. (22.5 percent by weight).
  • the grease has a solution temperature yof 370 F.
  • the piping arrangement 20, 21, 22 and 23 was preheated to about 420 F.
  • the contactor was pressured with air from line 19 such that the soap-oil mixture was forced Ilthrough the piping arrangement to a single high-pressure nozzle 24.
  • the temperature of the mixture charged to the nozzle was 415-412 F.
  • the nozzle pressure was between 2200 and 2700 p.s.i.
  • the product was sprayed into and collected in a drum receiver 26 and passed to a Cornell Cold Grease Homogenizer to remove air. Characteristics of the grease so obtained are shown in Table -I following where-in it is identified as Grease Example No. l. Several related products are shown in the same table.
  • EXAMPLE 5 This involves the preparation of a lithium soap grease composed of lithium l2-hydroxy stearato (8 pounds; 8 percent by weight) and a naphthenic oil, 750 seconds S.U.S. at 100 F., (92 pounds; 92 Weight percent).
  • the grease has a solution temperature of 383 E
  • the piping arrangement 20, 21, 22 and 23 was preheated to about 375 F.
  • the contacter was pressured with air from line 19 such that the soapoil mixture was forced to high pressure pump 25. From the pump 25, the mixture passed through 21, 2?. and 23 to a single high-pressure nozzle 24.
  • the temperature of the mixture charged to the nozzle was Afrom 365-358 F. As the product was expressed [from the nozzle, its temperature was about 200 F.
  • the nozzle pressure was between 3100 and 3600 p.s.i.
  • the product was sprayed into and collected in a drum receiver which served as receiver 26.
  • the grease so obtained was smooth in texture and had the vfollowing characteristics.
  • Example 6 Micro penetration, initial 125 icro penetration, final 187 A #further illustration of the preparation of a grease of the type shown in Example 5 is identified in the tollowing tabulation as Example 6.
  • Soaps and oil at 250 F. were taken from storage 13 and 15, and were charged to contactor 10.
  • Lithium hydroxide monohydrate and Water were heated to 212 F. and charged to the contacter. The latter was closed, and the .materials were mixed and heated therein to 372 E. over a period of 11/2 hours.
  • the ycontactor was then vented by opening valved line 18.
  • the mixture in the contacter was removed through line as described in Example 5. 'The entire pipe system 2t) through 23 was heated to about 350 F.
  • the temperature of the mixture changed to a single high-pressure nozzle was 355 F.
  • Nozzle pressure was 300D-4500 p.s.i.
  • the iinal product was a firm, transparent grease of the following nature.
  • EXAMPLE 9 This example is given to illustrate a lithium grease composed of lithium stearate and lithium-12 hydroxystearate.
  • the vehicle used was dipropylene glycol dipelargonate.
  • Micro penetration, initial Micro penetration, inal 109 EXAMPLE 10 Illustrated here is a lithium stearate grease. Fifteen percent by Weight of such soap. Iwas used with percent by weight or di-propylene glycol dipelargonate. Operating conditions and characteristics ofthe product are 'given below:
  • EXAMPLE 1'1 Provided here is an illustration of a mixed base grease comprised of lithium and calcium stearates.
  • the grease was formed from lithium stearate (7 percent by Weight), calcium stearate (2 percent by Weight) and a naphthenic mineral oil having a ⁇ viscosity index of 10.
  • the grease has a solution temperature of 366 F. The procedure used was that which is described above in Example 6.
  • Micro penetration, initial 82 Micro penetration, final 2 EXAMPLE 12 This example shows calcium soap -greases in an ester vehicle, dipropylene glycol dipelargonate. Calcium acetate monohydrate, calcium caprylate and calcium stearato in the percent Weight balance respectively of 11.6, 8.0 and 3.7, were employed. The salt-soap content, therefore was 23.3 percent by weight. The balance was ester vehicle.
  • Oleaginous vehicles useful herein have been illustrated above by mineral oils and synthetic esters. lt yis to be understood, however, that other ⁇ oils of ⁇ lubricating viscosity can Ialso be used in the present invention. Typical of such vehicles are polymerized oleins, silicones, uorocarbons, periluoroalkyl ethers, esters of polybasic acids, esters of poly-alcohols and monocarb-oxylic acids, silicate esters, esters of phosphorus-containing acids, amines, etc.
  • Illustrative of such vehicles are: polypropylene, polypropylene glycol, di-(2-ethyl hexyl) sebacate, di-(2ethyl hexyl) adipate, ydibutyl phthalate, polyethylene glycol di- (2-ethyl hexoate), polymethylsiloxane.
  • the synthetic vehicles are most suitable for providing -greases for use in aircraft, since many of these greases retain their lubrieating value over a wide temperature range, from about F. to about 500 F.
  • the mineral oils and synthetic lubricants which can tbe used herein are characterized by a viscosity (S.U.V.) of ⁇ greater thw about 40 seconds at 100 F., preferably from about 60 to about 6000 seconds at 100 F.
  • S.U.V. viscosity
  • soaps of lithium, of lithium and calcium, and of calcium alone can be used in the present invention.
  • soaps of any metals useful in forming grease compositions can be used in the present invention.
  • soaps of one ⁇ or more metals of the following group can be used: sodium, potassium, lithium, calcium, barium, strontium, zinc, ⁇ aluminium, etc.
  • the method of making a grease which comprises: wetting a pre-formed soap thickening agent in a greaseforming quantity with an foil of lubricating viscosity, at a temperature between about 250 F. and the lower of the decomposition temperatures of the said agent and oil; subjecting the vresulting oil-soap mixture at a temperature Within the aforesaid range and at a pressure above about 1000 pounds per square inch, to mechanical atomization Iinto dispersed droplets, and Vinstantaneously contacting the droplets Adirectly with a substantially cooler surrounding atmosphere to eiect heat exchange thereof, thereby forming a grease.
  • soap thickening agent is a mixture of calcium salts and soaps.
  • soap thickening agent is a complex of calcium salts and soaps.

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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)
US51139A 1960-08-22 1960-08-22 Grease manufacture Expired - Lifetime US3108965A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2157207A1 (de) * 1970-11-18 1972-05-25 Esso Research and Engineering Co , Lmden, NJ (V St A ) Schmierfett

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2735815A (en) * 1956-02-21 Preparation of soap-salt complexes
US2846392A (en) * 1953-10-21 1958-08-05 Exxon Research Engineering Co Metal soap-salt complexes and lubricants containing same
US2950249A (en) * 1957-09-13 1960-08-23 Socony Mobil Oil Co Inc Grease-making process involving mechanical atomization
US2950248A (en) * 1954-09-24 1960-08-23 Socony Mobil Oil Co Inc Grease manufacture including mechanical atomization of the charge

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2735815A (en) * 1956-02-21 Preparation of soap-salt complexes
US2846392A (en) * 1953-10-21 1958-08-05 Exxon Research Engineering Co Metal soap-salt complexes and lubricants containing same
US2950248A (en) * 1954-09-24 1960-08-23 Socony Mobil Oil Co Inc Grease manufacture including mechanical atomization of the charge
US2950249A (en) * 1957-09-13 1960-08-23 Socony Mobil Oil Co Inc Grease-making process involving mechanical atomization

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2157207A1 (de) * 1970-11-18 1972-05-25 Esso Research and Engineering Co , Lmden, NJ (V St A ) Schmierfett

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