US2678918A - Production of anhydrous soda base lubricating greases - Google Patents

Production of anhydrous soda base lubricating greases Download PDF

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Publication number
US2678918A
US2678918A US655887A US65588746A US2678918A US 2678918 A US2678918 A US 2678918A US 655887 A US655887 A US 655887A US 65588746 A US65588746 A US 65588746A US 2678918 A US2678918 A US 2678918A
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Prior art keywords
grease
soap
soda
greases
molecular weight
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Arnold A Bondi
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Shell Development Co
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Shell Development Co
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Priority to GB7740/47A priority patent/GB639203A/en
Priority to DEN1736A priority patent/DE938087C/de
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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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    • 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
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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
    • C10M2203/102—Aliphatic fractions
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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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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • 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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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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    • C10M2207/283—Esters of polyhydroxy compounds
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    • C10M2207/286—Esters of polymerised unsaturated acids
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    • C10M2207/40—Fatty vegetable or animal oils
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/40—Fatty vegetable or animal oils
    • C10M2207/404—Fatty vegetable or animal oils obtained from genetically modified species
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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
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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
    • C10M2209/106—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing four 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
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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
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    • C10N2010/00—Metal present as such or in compounds
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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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

Definitions

  • This invention relates to the production of lubricants and, more particularly, to substantially anhydrous soda soap greases containing small amounts of the higher polyalkylene glycols, that is, those above the trialk 'lene glycol, said glycols being exemplified by the polyethylene glycols, the polypropylene glycols, the polybutylene glycols, the polyamylene glycols, and the polyhexylene glycols.
  • the soda soap-greases of the present invention may contain a small amount of the liquid polyalkylene glycols having a molecular weight varying between about 200 and about 600, or a solid polyalkylene glycol having a molecular weight varying from about 1000 to 7000.
  • soda soap greases are-exceedingly sensitive to rapid cooling from a highly heated liquid state to a solid state. This has made it necessary to slowly cool the grease from its hot liquid state adjacent its melting point and higher in a period usually varying from 12 to 16 hours when cooled in layers of three inches to five inches in thickness, bleeding of the oil from the grease being inhibited during this cooling period.
  • quick cooling is accomplished, and bleeding is prohibited by incorporating in the grease a small amount of a higher polyalkylene glycol thereof having the character set forth and cooling in the presence thereof, the percentage of polyalkylene glycol present in the grease ranging from about 0.05% to 1% and preferably from 0.1% to 0.25% or 0.3% taken on the weight of the grease, said cooling being preferably in thin layers averaging fromto about in thickness. Greater amounts may be used but are not necessary to accomplish the purpose of the present invention. Desirably, the amount of the polyalkylene glycol incorporated in the grease should not materially decrease the melting point of the grease. Some decrease in the melting point of the grease for certain purposes will not be harmful.
  • the higher molecular weight polyalkylene glycols of the character herein referred to and, more particularly, the polyethylene glycols are added to lubricating greases of the anhydrous soda soap or soda base type during or after the cooking operation, and the resulting greases may be cooled from their liquid state at extremely rapid rates of the'character herein set forth without any deleterious effect on the physical or chemical properties of the grease, that is, there is no bleeding of the grease, the latter, under certain circumstances, becoming completely reversible.
  • Example 1 The following ingredients are mixed and cooked:
  • Example 2 The following ingredients are mixed and cooked following the procedure set forth in Example 1:
  • the grease had an ASTM penetration, after 60 strokes, of 305 decimillimeters, and after 300 strokes, 328 decimillimeters.
  • the grease assumed a temperature of about 95 F. within twenty minutes after pouring into the cooling pans, the surrounding air having a temperature of about 75 F.
  • a grease will cool from between 300 F. and 400 F. to about F. to F. in about five to twenty minutes when a specimen of the grease is poured on a steel plate at a temperature varying between 300 F. and 500 F.
  • the above set forth grease containing from .05% to 1% of a polyalkylene glycol, is a completely reversible grease, thereby distinguishing from all prior known soda base greases which, although they were mechanically stable and, had a relatively high melting point, were not reversible; that is, the prior art soda base greases could not be melted and cooled for a plurality of cycles, as for example, four to fifteen cycles and/or at any rate of cooling without change in texture and mechanical properties.
  • the method of incorporation of the polyalkylene glycols into the soda base greases is not limited to the cooking procedure disclosed in connection with Examples 1 and 2, said procedure being set forth primarily for the purpose of illustration and not by way of limitation, said batches being illustrative of standard batches, and the procedure being illustrative of the standard procedure used in the production of anhydrous soda soap or soda base greases. Therefore, in carrying out the present invention, any of the prior art grease cooling procedures may be employed, and the grease may be mixed and cooked through a wide range of temperatures varying from room temperature; that is, about 68 F. to about 500 F.
  • the polyalkylene glycols in percentages ranging from 0.01% to may be incorporated prior to cooking, or during cooking, or they may be incorporated in a soda base grease which has already been prepared and cooled by melting the grease and mixing it with a polyalkylene glycol of the character herein set forth, namely, one having a molecular weight between 200 and 7000.
  • polyalkylene glycols are oil soluble. They may be, therefore, dissolved, directly in the oil. However, the polyalkylene glycols may be brought into aqueous solution, or an aqueous emulsion may be formed thereof and the grease cooked in the presence of the aqueous emulsion provided all of the water is substantially eliminated or evaporated out of the grease during the cooking operation or thereafter so that there is produced a substantially anhydrous soda soap or soda base grease.
  • a substantially anhydrous soda soap grease is meant one that has a water-content of less than about 0.2% to 25% based on the weight of the grease and preferably has a water-content varying from less than .01% to 0.1%.
  • anhydrous soda basegreases' may-be quikly cooled as herein set forth.
  • Example- 4 The following batch was. mixed:
  • the samebatch of constituents was mixed with ofpolyethylene *glycol having'an-average molecular weight of 1500; andthen cooked" 61-. in the usual manner. There: was; produced; grease having an ASTM penetration. afterrfip' strokes, o;f. 220 decimillimeters which increased in softness, after 9 hoursin-ashell roller tester only from 74 to 104 decimillimeters penetration as determined using the Shell Microcone.
  • the fatty acid constituent which may be a saturated fatty acid or an unsaturated fatty acid, which may be used in carrying out the present invention includes stearic acid, l2-hydroxy stearic acid, 9, 10-dihydroxy stearic acid, 4-hydroxy palmitic acid; iso stearic acid, iso-palmitic acid, 12-hydroxy 9- oleic acid (ricinoleic acid), oleic acid, lineoleic acid, hydrogenated fish oil fattyacids, palm oil fatty acids, cotton seed oil' fatty acids.
  • abietic acid, and/or the corresponding glycerides thereof, and/or naphthenic acids maylee-incorporated in the grease making batch.
  • rated fatty acids containing up to 32 carbon atoms and usually from 14 to 32. carbon atoms;
  • the saponifiable. constituent of the grease making batch may be a vegetable oil or an animal oil or fat usually, used in the production of anhydrous soda base. greases; In short, any of theprior artsaponifiable media may be used which are set forth in. Klemgards book entitled, Lubricating Greases; Their Manufacture and Use" (1937) published by the Reinhold Publishing Company, New York;
  • the saponifying medium may be sodium-hydrox: ide or metallic sodium, and the present invention may be carried out when. using metallic, sodium inaccordance with the disclosure of my.
  • polyajlkyle ene glycols having between 2 and 6 carbon atoms 5 in the alkylene groups are effective in carrying:.
  • the average molecular weight of the polyethylene glycols used in carrying out the present invention may. vary from 200 to 7000 or 400 to-7000, the preferred molec ular weiglit varyingfrom. 1000 to 4000; It appears that the most effective average molecular weight is about 1500.
  • Polyethylene glycol has the following formula:
  • the polyethylene glycol may be replaced by polymerized polypropylene glycol or polymerized polybutylene glycol, said glycols having an average molecular weight in excess of 200, and usually between 200 and 7000.
  • the greases of the present invention may carry a sodium soap in the amount in which it is customarily present in sodium soap greases, the prior art greases being well set forth in Klemgards book previously referred to. More specifically, the soda soap greases of the present invention may carry from 1% to 50% of a sodium soap, but more usually carry from 1% to 15%, and, preferably, carry from 3.5% to l /2%, or
  • polyethylene glycol 400 consists of various glycols varying from a minor portion of tetraethylene glycol with increasing amounts of nona ethylene glycol and then increasing up to the pentadecaethylene glycol. Therefore, it is the average molecular weight which is specified and wherein the present specification polyalkylene glycols or polyethylene glycols are referred to, they define the higher glycols having an average molecular weight in excess of 200 and preferably in excess of 400, those with an average molecular weight in excess of 1000 being very effective in carrying out the present invention.
  • an anhydrous reversible soda base lubricating grease said grease containing from 1% to 50% of a soda soap and, preferably, between 3.5% to of a soda soap base.
  • the anhydrous grease contains from about .01% to 1% of a polyalkylene glycol of the character set forth.
  • the anhydrous grease becomes completely reversible when the amount of polyalkylene glycol is around 05%. With all amounts of the polyalkylene glycol, the grease becomes bleedless, and when the grease has present between about .05% to 1% or greater amounts, the grease is capable of being quickly cooled within the spirit of the present invention.
  • the invention in one of its forms comprises cooling a hot fluid anhydrous sodium soap lubricating grease to its solid state in the presence of a polyalkylene glycol having an average molecular weight in excess of 200, the amount of the polyalkylene glycol ranging from .01% to about 1%.
  • the present invention is also directed to a method of preventing bleeding of oil from an anhydrous lubricating grease containing a lubricating oil base and a sodium soap by incorporating in the grease from .01% to about 1% of a polyalkylene glycol having an average molecular weight in excess of 200.
  • the method is also directed to accelerating the cooling of a hot liquid sodium soap lubricating grease through a cooling range of at least 200 F. to a solid state adjacent room temperature and in the absence of any bleeding comprising incorporating in the grease a polyalkylene glycol in an amount greater than .05%, said polyalkylene glycol having an average molecular weight in excess of 200.
  • a hot grease in layers of about to about 1" will cool from about 350 F. or a little higher to a room temperature of F. in less than two hours; that is, between 30 seconds and two hours.
  • the raw materials are cooked together in the presence of the polyalkylene glycol, the latter may be added to the cooled grease by agitation, and then the mass may be heated to above 300 F. and allowed to cool. This will produce a grease which does not bleed and which can be quickly cooled in layers of A to 1" in less than 2 to 4 hours.
  • any of the prior art aluminum or calcium soaps there may be introduced therein small amounts of any of the prior art aluminum or calcium soaps, and by small amounts is meant less than 2% of any prior art aluminum soap or less than 2% of any prior art calcium soap, or the amount of prior art aluminum soap or prior art calciumsoap in the grease together may be less than 2%, and the properties of the grease which are conferred thereon due to the use of the polyalkylene glycols will be retained by the grease. More specifically, the amount of the aluminum soap and/or calcium soap may vary between 0.1% to 2% taken on the weight of the grease.
  • said grease can be mixed when cooled with any amount of aluminum soap grease or calcium soap grease.
  • any amount of aluminum soap grease or calcium soap grease there may be incorporated into the soda base grease 1% to 70% of aluminum soap grease or 1% to 70% of a calcium soap grease, or mixtures thereof, said greases being incorporated into the cold sodium soap grease.
  • Any of the polyalkylene glycols herein broadly and specifically set forth may be mixed with each other in any proportion and used in the place of a single polyalkylene glycol.
  • the anhydrous soda base greases usually contain less than .25% of water.
  • An anhydrous soda base lubricating grease containing .05% to about 1% of a polyethylene glycol having an average molecular weight in excess of 200, said percentage range being taken on the weight of the grease.
  • An anhydrous soda base lubricating grease containing to about 1% of a polyethylene glycol having an'average molecular weight varying between about 200 and about 7000, said percentage range being taken on the weight of the grease.
  • An anhydrous soda base lubricating grease containing from 05% to about 1% of a polyethylene glycol having an average molecular weight varying between about 1000 and about 4000, said percentage range being taken on the weight of the grease.
  • An anhydrous reversible soda base lubricating grease containing about 1% to 50% by weight of a soda soap and about 0.01% to about 1% of a polyethylene glycol having a molecular weight greater than 200.
  • An anhydrous reversible soda base lubricat ing grease containing .1% to .3% of a polyalkylene glycol having an average molecular weight in excess of 200, said percentage range being taken on the weight of the grease.
  • An anhydrous bleedless reversible soda base lubricating grease containing about 0.01% to about 1% of a polyalkylene glycol in which the total carbon atoms present in the alkylene groups I 8.
  • a substantially anhydrous bleedless soda base lubricating grease containing 01% to 05% of a polyalkylene glycol having an average molecular weight in excess of 200, said percentage range being taken on the weight of the grease.
  • a substantially anhydrous bleedless soda base lubricating grease containing 01% to 05% of a polyalkylene glycol having an average molecular weight varying between 400 and Z000, said percentage range being taken on the weight of the grease.
  • An anhydrous bleedless soda base lubricating grease containing .1% to .5% of a polyalkylene glycol in which the total carbon atoms present in the alkylene groups varies from 2 to 6 inclusive, said polyalkylene glycol having a molecular weight in excess of 200, said percentage range being taken on the weight of the grease.
  • An anhydrous bleedless soda base lubricating grease containing .1% to .5% of a polyethylene glycol in which the total carbon atoms present in the ethylene groups varies from 2 to 6 inclusive, said polyethylene glycol having a molecular weight in excess of 200, said percentage range being taken on the weight of the grease.
  • An anhydrous bleedless lubricating grease containing a grease producing amount of a sodium soap of 12-hydroxy stearic acid and having present 01% to 05% of a polyalkylene glycol in which the total carbon atoms present in the alkylene groups varies from 2 to 6 inclusive, said polyalkylene glycol having a molecular weight in excess of 200, said percentage range being taken on the weight of the grease.
  • a lubricating grease composition consisting essentially of mineral lubricating oil thickened to a grease consistency by the sodium soap of substantially saturated higher fatty acids and containing about 0.1% of polyethylene glycol having a molecular weight of about 1000.
  • a soda soap base lubricating grease containing 0.05% to about 1% of a polyethylene glycol having an average molecular Weight in excess of 200, said percentage range being taken on the weight of the grease.
  • a lubricating grease composition comprising mineral lubricating oil thickened to a grease consistency by the sodium soap of substantially saturated higher fatty acids and containing about 0.05% to about 1% of polyethylene glycol having an average molecular weight between about 200 and about 7000.

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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)
US655887A 1946-03-20 1946-03-20 Production of anhydrous soda base lubricating greases Expired - Lifetime US2678918A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
NL67825D NL67825C (enrdf_load_stackoverflow) 1946-03-20
US655887A US2678918A (en) 1946-03-20 1946-03-20 Production of anhydrous soda base lubricating greases
GB7740/47A GB639203A (en) 1946-03-20 1947-03-20 Improvements in the manufacture of substantially anhydrous sodium soap lubricating greases
DEN1736A DE938087C (de) 1946-03-20 1950-08-31 Praktisch wasserfreie Natriumseife enthaltende Schmierfette auf Mineraloelbasis

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US655887A US2678918A (en) 1946-03-20 1946-03-20 Production of anhydrous soda base lubricating greases

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US2678918A true US2678918A (en) 1954-05-18

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US655887A Expired - Lifetime US2678918A (en) 1946-03-20 1946-03-20 Production of anhydrous soda base lubricating greases

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US (1) US2678918A (enrdf_load_stackoverflow)
DE (1) DE938087C (enrdf_load_stackoverflow)
GB (1) GB639203A (enrdf_load_stackoverflow)
NL (1) NL67825C (enrdf_load_stackoverflow)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2820762A (en) * 1952-04-01 1958-01-21 Exxon Research Engineering Co Mixed hydroxy fatty acid-unsaturated fatty acid thickened grease compositions
US2872416A (en) * 1953-09-30 1959-02-03 Exxon Research Engineering Co Anti-friction bearing grease and preparation thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2850454A (en) * 1952-12-01 1958-09-02 Exxon Research Engineering Co Production of greases by alkali fusion of materials containing hydroxy fatty acid and glycerine radicals

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2398173A (en) * 1944-01-29 1946-04-09 Standard Oil Co Lithium soap greases

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2398173A (en) * 1944-01-29 1946-04-09 Standard Oil Co Lithium soap greases

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2820762A (en) * 1952-04-01 1958-01-21 Exxon Research Engineering Co Mixed hydroxy fatty acid-unsaturated fatty acid thickened grease compositions
US2872416A (en) * 1953-09-30 1959-02-03 Exxon Research Engineering Co Anti-friction bearing grease and preparation thereof

Also Published As

Publication number Publication date
DE938087C (de) 1956-01-19
NL67825C (enrdf_load_stackoverflow)
GB639203A (en) 1950-06-21

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