US2846391A - Process for sodium soap-salt thickened lubricating greases containing sodium phosphate - Google Patents

Process for sodium soap-salt thickened lubricating greases containing sodium phosphate Download PDF

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Publication number
US2846391A
US2846391A US293671A US29367152A US2846391A US 2846391 A US2846391 A US 2846391A US 293671 A US293671 A US 293671A US 29367152 A US29367152 A US 29367152A US 2846391 A US2846391 A US 2846391A
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Prior art keywords
grease
soap
oil
salt
temperature
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US293671A
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English (en)
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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 BE520539D priority Critical patent/BE520539A/xx
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Priority to US293671A priority patent/US2846391A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M5/00Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085Phosphorus oxides, acids or salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/122Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
    • C10M2215/065Phenyl-Naphthyl amines
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/14Containing carbon-to-nitrogen double bounds, e.g. guanidines, hydrazones, semicarbazones
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/26Amines
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/02Groups 1 or 11
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

Definitions

  • the present invention relates to improvements in lubricating greases and methods for their production. More specifically it relates to an improved process for preparing lubricating greases which are stable at high temperatures and under operating conditions where high rates of shear are involved. It has particular application to lubricating greases which are used in anti-friction bearings such as ball and roller bearings.
  • sodium phosphate is a desirable additive for lubricating greases.
  • S0- dium or potassium silicate, borate or carbonate has been used in an analogous manner.
  • the present invention is based on the discovery that a superior product may be prepared by processing it in a particular manner so as to incorporate the phosphate or analogous salt into the grease either as an element of a complex soap-salt system or, at any rate, in such a manner that no detectable crystals of salt are found.
  • the process of the present invention involves saponifying a suitable fatty oil, preferably rapeseed oil, or mixtures of fatty acids and glycerine, etc. at a moderate temperature in the presence of a portion only of the lubricating oil which is eventually to be used in the grease. Thereafter the saponified mixture is heated to a relatively very high temperature, i. e. 475 to 575 F., to cause the glycerine released upon saponification to react with the saponifying agent, for example, according to the Cannizzaro reaction. The glycerine apparently is converted to acrolein which in turn undergoes a reaction which results in a low molecular weight salt product.
  • a suitable fatty oil preferably rapeseed oil, or mixtures of fatty acids and glycerine, etc.
  • a preferred product made according to the present invention will consist of about 65 to by weight of lubricating oil, preferably a mineral base oil.
  • the soap content of the grease is between 10 and 35% by weight, preferably of soda soap, and the phosphate content is from about "0.5 to about 3%.
  • Conventional additives may be employed such as 0.25 to 2% of a phenyl naphthylamine as antioxidant and a similar quantity of an oil soluble sulfonate to give further protection against rust where that is of major importance.
  • 0.1 to 1% of a good metal deactivator may be used, for example di-salicylal-propylene-diamine.
  • the grease of the present invention will be prepared initially with a relatively high soap content. It may be oiled back subsequently by adding 75 to of its weight of lubricating oil. Thereafter the oiled back product is stabilized against oil separation and against mechanical breakdown in service by subjecting the composition to high rates of shear in a mechanical worker, homogenizer or mill. Suitably homogenized grease may contain as little as6% soap. This particular aspect of the process forms no part of the present invention. Ordinarily, mineral base oils are preferred throughout but the invention also contemplates the use of synthetic esters, polyglycols and other synthetic oils which are well known to those skilled in the art.
  • the saponification step at least should be carried out in the presence of an inert material such as mineral base oil to which the synthetic oil, if employed, may be added later. It is also desirable, ordinarily, to saponify the fatty oil in the presence of a relatively small part of the total oil used, usually not more than half and preferably somewhat less than half, for example about a third of the total lubricating oil content. Additional oil, of mineral or synthetic type, is added to the concentrate thus formed.
  • an inert material such as mineral base oil to which the synthetic oil, if employed, may be added later. It is also desirable, ordinarily, to saponify the fatty oil in the presence of a relatively small part of the total oil used, usually not more than half and preferably somewhat less than half, for example about a third of the total lubricating oil content. Additional oil, of mineral or synthetic type, is added to the concentrate thus formed.
  • the grease was prepared by the following procedure. Rapeseed oil, about one-third of the mineral oil, and
  • Short fiber Short fiber Short fiber Light yellow Light yellow Dark brown.
  • the sodium sulfonate concentrate were charged to a fire heated grease kettle and warmed to about 150 F. This temperature should be between and 200 F., the narrower limits of and F. being preferred. When this temperature range was reached a 50% aqueous solution of sodium hydroxide was added in quantitics suflicient to saponify the rapeseed oil, react with the glycerine, and still leave an excess sufficient to react with the proportions of the acid of phosphorus mentioned above, that is 1.33%, though quantities of 0.5 to 3% or so of the acid may be used.
  • Example II The product of Example I was diluted by adding an equal weight of mineral base lubricating oil of about 50 S. S. U. viscosity at 210 F. and a viscosity index of about 60. The oil and grease were mixed together and homogenized by passing the mixture twice through the Manton-Gaulin homogenizer at a pressure of 3,000 p. s.:i. g. The resulting product was smooth and almost transparent with a light yellow color.
  • the properties iii) Various modifications may be made in process and product as will be self-evident to those skilled in the art.
  • the preferred temperature ranges for the process are those listed above but they may be varied in some degree and cooling of the grease may be accomplished in various ways known to the art.
  • Various conventional additives such as anti-oxidants, thickeners, viscosity index improving agents, pour point depressants, and 'the like may be present as will be obvious to those skilled in the art.
  • a grease-forming mixture of rapeseed oil, sodium hydroxide and an inert mineral lubricating oil is heated after saponification and dehydration to-a temperature in the range of 475 to 575 F. to cause the glycerine released by saponification and decomposition products of the-glycerine to react with said sodiumhydroxidc;
  • the improved method of incorporatingtrisodium phosphate into said grease which comprises maintaining in the reactants an excess of said sodium hydroxide above the quantity required for saponification and reaction with the glycerine and decomposition products thereof, adding to the reactionmixture at a temperature above 450 F. before appreciably cooling the grease in the range of 0.5 to 3.0 weight percent of orthophosphoric acid, forming thereby from the acid and excess alkali trisodium phosphate in such a form that no detectable crystals of the salt exist.

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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)
US293671A 1952-06-14 1952-06-14 Process for sodium soap-salt thickened lubricating greases containing sodium phosphate Expired - Lifetime US2846391A (en)

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Application Number Priority Date Filing Date Title
BE520539D BE520539A (US06649357-20031118-C00005.png) 1952-06-14
US293671A US2846391A (en) 1952-06-14 1952-06-14 Process for sodium soap-salt thickened lubricating greases containing sodium phosphate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3318807A (en) * 1963-05-13 1967-05-09 Texaco Inc Lubricating greases containing finely divided inorganic metal salts and method of preparation therefor

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2265791A (en) * 1939-04-06 1941-12-09 Standard Oil Dev Co Grease composition and method for making same
US2360631A (en) * 1942-12-09 1944-10-17 Standard Oil Dev Co Lubricant
US2413121A (en) * 1944-03-20 1946-12-24 Standard Oil Co Greases
US2417431A (en) * 1945-03-31 1947-03-18 Union Oil Co Lubricants
US2417432A (en) * 1945-03-31 1947-03-18 Union Oil Co Lubricants
US2417430A (en) * 1945-03-31 1947-03-18 Union Oil Co Lubricants
US2417429A (en) * 1945-04-16 1947-03-18 Union Oil Co Complex basic soap greases
US2417428A (en) * 1946-09-19 1947-03-18 Union Oil Co Lubricating composition
US2417433A (en) * 1945-04-23 1947-03-18 Union Oil Co Lubricating composition
US2468099A (en) * 1947-10-01 1949-04-26 Standard Oil Dev Co High-temperature grease
US2468098A (en) * 1948-02-18 1949-04-26 Standard Oil Dev Co Grease composition
US2513680A (en) * 1949-01-18 1950-07-04 Socony Vacuum Oil Co Inc Lime base grease
US2595161A (en) * 1950-05-24 1952-04-29 Standard Oil Dev Co Lubricating composition

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2265791A (en) * 1939-04-06 1941-12-09 Standard Oil Dev Co Grease composition and method for making same
US2360631A (en) * 1942-12-09 1944-10-17 Standard Oil Dev Co Lubricant
US2413121A (en) * 1944-03-20 1946-12-24 Standard Oil Co Greases
US2417431A (en) * 1945-03-31 1947-03-18 Union Oil Co Lubricants
US2417432A (en) * 1945-03-31 1947-03-18 Union Oil Co Lubricants
US2417430A (en) * 1945-03-31 1947-03-18 Union Oil Co Lubricants
US2417429A (en) * 1945-04-16 1947-03-18 Union Oil Co Complex basic soap greases
US2417433A (en) * 1945-04-23 1947-03-18 Union Oil Co Lubricating composition
US2417428A (en) * 1946-09-19 1947-03-18 Union Oil Co Lubricating composition
US2468099A (en) * 1947-10-01 1949-04-26 Standard Oil Dev Co High-temperature grease
US2468098A (en) * 1948-02-18 1949-04-26 Standard Oil Dev Co Grease composition
US2513680A (en) * 1949-01-18 1950-07-04 Socony Vacuum Oil Co Inc Lime base grease
US2595161A (en) * 1950-05-24 1952-04-29 Standard Oil Dev Co Lubricating composition

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3318807A (en) * 1963-05-13 1967-05-09 Texaco Inc Lubricating greases containing finely divided inorganic metal salts and method of preparation therefor

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