US2182137A - Soda soap grease - Google Patents

Soda soap grease Download PDF

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US2182137A
US2182137A US123491A US12349137A US2182137A US 2182137 A US2182137 A US 2182137A US 123491 A US123491 A US 123491A US 12349137 A US12349137 A US 12349137A US 2182137 A US2182137 A US 2182137A
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grease
mineral oil
soda soap
soap
acids
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US123491A
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Vernon L Ricketts
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Shell Development Co
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Shell Development Co
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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
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/18Natural waxes, e.g. ceresin, ozocerite, bees wax, carnauba; Degras
    • 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
    • C10M2207/02Hydroxy compounds
    • C10M2207/021Hydroxy compounds having hydroxy 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
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/141Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings 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
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/142Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic
    • 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
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/144Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/146Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings having carboxyl groups bound to carbon atoms of six-membeered aromatic rings having a hydrocarbon substituent 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/16Naphthenic 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
    • C10M2211/00Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/04Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen, halogen, and oxygen
    • C10M2211/044Acids; Salts or esters thereof
    • 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
    • C10M2215/26Amines
    • 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
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/04Groups 2 or 12
    • 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
    • C10N2010/06Groups 3 or 13
    • 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
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
    • 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

  • a lubricant which is suitable for use at high temperatures, and preventing or reducing leakage of the lubricant from the bearings at high temperatures. It is a further object of the invention to increase the yield of a grease of the type described in proportion to the soap content, while maintaining and often improving the stability of the grease at normal and at high temperatures. Still another object of the invention is to improve the stability of such a grease, as indicated by freedom from granulation, by absence of any tendency to bleed or separate either during manufacture or later in storage, and by resistance to breakdown from mechanical stirring or beating. Other objects will be apparent from the following specification.
  • a metal salt of an organic carboxylic acid containing an arcmatic ring may be employed, but I prefer to employ salts of alkali metals or alkaline earth metals, particularly sodium.
  • the negative radical of the salt may have the formula R.C(O) .0 where R represents an organic radical containing an aromatic ring which may or may not be substituted with hydrocarbon and/or non-hydrocarbon groups.
  • the acid residue may be linked directly to the aromatic nucleus, or it may be linked thereto through an aliphatic or oxy-aliphatic chain, which may be saturated CnH2nor unsaturated .CnH2n2-, and which may be substituted with hydrocarbon and/or non-hydrocarbon groups.
  • the negative radical may, for example, contain one or more of the following substituents: Halogen, such as C1; amines, as NI-Iz, NHR or NRz (which R represents an aliphatic chain) aliphatic chains, such as CHa, CzHs; and hydroxyl, such as OH and ROH.
  • the radical R may, moreover, contain additional carbonyl-containing radicals, such as --C O OH, CHO, C(O) .ONH4 or -C(( .OM, wherein M represents a metal.
  • salts apparently act as peptizing agents for the soda soap, and result in an effective dispersion of soap in oil, the formation of line lattices contributing to increased yields and improved stabilities.
  • the salts are, moreover, preferably resistant to solution in oil, this property being of especial value in increasing the melting point of the grease.
  • Suitable salts are: metal benzoate, CsHsC (O) .OM, metal cinnamate,
  • metal salicylate HO
  • metal xylate CH3 2C6H3C(0) .OM
  • metal vanillate CI-I30
  • M represents a metal, such as sodium, potassium, calcium, zinc, and aluminum, but preferably sodium.
  • the salt present in the composite grease, according to the present invention is preferably present in concentrations between 0.1% and 6% by weight, although higher concentrations may also be employed.
  • the salt may be formed apart from the step of saponification of the aliphatic material employed for the grease base, and added to the soap, either before or after admixture to mineral oil, and while the soap is heated; it may, however, also be formed in the same operation, as is explained below in the specific examples.
  • the soda soap may constitute between about 2.5% and 39% of the composite grease.
  • soda soap designates sodium salts of carboxylic acids containing at least 10 carbon atoms, as, for examples, salts of higher fatty acids, of naphthenic acids, and of mineral oil sulfonates. While any of the commonly used saponiflable materials may be employed for the production of the soda soap, such as fats and fatty acids, it was found that best results are obtained by employing materials having aliphatic acid residues containing over 20 carbon atoms. Thus, the use of beeswax or degras is preferred over the use of such materials as spermaceti or palm oil.
  • saponifiable materials consist entirely or mainly of aliphatic acids or of esters of aliphatic acids of between 10 and 20 carbon atoms
  • beeswax or degras or a similar material to the extent of at least 40% of the total saponiflables.
  • the use of tallow, spermaceti or similar materials without the addition of materials containing higher aliphatic acids or acid residues often results in the production of a grease having a brittle texture, and may even cause granulation due to soap and oil separation.
  • the mineral oil constitutes between about 61% and 97.7% of the composite grease.
  • a wide variety of viscous mineral oils may be employed for this purpose. For example, oils having viscosities between about 50 seconds and 250 seconds Say. Univ. at 210 F. may be used. Since, however, the greases, according to the present invention, generally have higher melting points, they must be compounded at elevated temperatures, as, for example, between 500 F. and 620 F., so that because of a fire hazard special precautions must be taken if oils of low flash points, such as those having viscosities less than 100 sec. Say. Univ. at 210 F. are employed. When oils having viscosities above 100 seconds are employed, no special precautions are generally necessary, but it is desirable to carry out the operation in an atmosphere of carbon dioxide or nitrogen when less viscous oils are used.
  • the grease may, for example, be prepared in the following manner: Approximately 0.5 to 1.0 volumes of the mineral oil and the calculated amount of 45 B. caustic soda are added to the melted saponifiables, the quantity of caustic soda depending upon the saponiilcation numbers of,
  • the fats, waxes, etc. for any specific formula, and also upon the percentage of the metal salt which is to be employed.
  • the resulting mixture is heated while stirring to a temperature of approximately 250" F. to 325 F., for a period sufflcient to cause saponification, usually between thirty minutes to one hour.
  • the material containing the negative radical of the metallic salt to be employed such as, for example, benzoic acid, benzaldehyde, or ammonium benzoate, etc., is dissolved in a large body of the oil, and the resulting solution is then added slowly to the soap base while stirring. The balance of the mineral temperatures.
  • Example I Two greases, designated below as A and-B, were compounded in the manner described above em Per cent Per cent Beeswax l0. 0 l0. 0 7 acid 2. 0 0
  • the grease C was, similar in stability and appearance to the grease A; grease D was, however, slightlygranular and curdled.
  • the properties of the two greases are given below:
  • the grease compositions of the present invention are useful in solving a large number of lubrication problems in which the high melting points and superior stability of lubricants of the present invention contribute to reduced leakage, more eflicient lubrication, and reduced maintenance costs.
  • a few examples of such applications are: transmission and difierential lubrication, particularly in automobiles, automotive chassis lubrication, universal joint lubrication, roller bearing lubrication, ball bearing lubrication, rocker arm lubrication, particularly in airplanes, journal lubrication in railway equipment, in lumber mills, and in other industrial plants.
  • the properties of the grease are further apparent from the following tests: 16 grams of grease A of Example I were charged into a ball bearing machine comprising an unloaded ball bearing mounted on a vertical spindle, and surrounded by a grease cup extending several centimeters above the plane of the bearing. The machine was operated for 20 minutes at 4600 R. P. M. without the application of external heat, the temperature rising spontaneously to about 150 F. No pronounced tendency for the lubricant to form fibers or work out of the bearing was noted. At the completion of the test the grease remained unchanged in appearance and structure. There was no evidence of breakdown or of separation of oil and soap.
  • a soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of an alkali metal salt of an organic carboxylic acid Y containing an aromatic ring to prevent bleeding.
  • a soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of sodium benzoate to prevent bleeding.
  • a soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of sodium salicylate to prevent bleeding.
  • a soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of sodium cinnamate to prevent bleeding.
  • a soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5 and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids,
  • naphthenic acids and mineral oil sulphonic acid said grease containing between .1 and 6% of an alkali metal salt of an organic carboxylic acid containing an aromatic ring to prevent bleeding.
  • a soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5.and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of sodium benzoate to prevent bleeding.
  • a soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5 and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of sodium salicylate to prevent bleeding.
  • a soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5 and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of sodium cinnamate to prevent bleeding.
  • a soda soap grease comprising a viscous mineral oil and a soda soap of a higher fatty acid, said grease containing a minor proportion of an alkali metal salt of an organic carboxylic acid containing an aromatic ring to prevent bleeding.
  • a soda soap grease comprising viscous mineral oil and a soda soap of an acid selected from a group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acids, at least 40% of said soap consisting of a soda soap of saponifiable material of the type of beeswax, which is rich in fatty acids containing more than 20 carbon atoms, said grease containing a minor proportion of an alkali metal salt of an organic carboxyllc acid containing an aromatic ring to prevent bleeding.

Description

Patented Dec. 5, 1939 UNITED STATES PATENT OFFICE SODA SOAP GREASE Vernon L. Ricketts, Martinez, Calil'., assignor to Shell Development Company, San Francisco, Calif., a corporation of Delaware No Drawing. Application February 1, 1937,
Serial No. 123,491
14 Claims.
the simple admixture of mineral oil to soda soaps,
thereby producing a lubricant which is suitable for use at high temperatures, and preventing or reducing leakage of the lubricant from the bearings at high temperatures. It is a further object of the invention to increase the yield of a grease of the type described in proportion to the soap content, while maintaining and often improving the stability of the grease at normal and at high temperatures. Still another object of the invention is to improve the stability of such a grease, as indicated by freedom from granulation, by absence of any tendency to bleed or separate either during manufacture or later in storage, and by resistance to breakdown from mechanical stirring or beating. Other objects will be apparent from the following specification.
In accordance with the present invention, these and other objects are achieved by incorporating into the grease a small quantity of a metal salt of an organic carboxylic acid containing an arcmatic ring. Salts of both light and heavy metals may be employed, but I prefer to employ salts of alkali metals or alkaline earth metals, particularly sodium. The negative radical of the salt may have the formula R.C(O) .0 where R represents an organic radical containing an aromatic ring which may or may not be substituted with hydrocarbon and/or non-hydrocarbon groups. The acid residue may be linked directly to the aromatic nucleus, or it may be linked thereto through an aliphatic or oxy-aliphatic chain, which may be saturated CnH2nor unsaturated .CnH2n2-, and which may be substituted with hydrocarbon and/or non-hydrocarbon groups.
The negative radical may, for example, contain one or more of the following substituents: Halogen, such as C1; amines, as NI-Iz, NHR or NRz (which R represents an aliphatic chain) aliphatic chains, such as CHa, CzHs; and hydroxyl, such as OH and ROH.- The radical R may, moreover, contain additional carbonyl-containing radicals, such as --C O OH, CHO, C(O) .ONH4 or -C(( .OM, wherein M represents a metal.
These salts apparently act as peptizing agents for the soda soap, and result in an effective dispersion of soap in oil, the formation of line lattices contributing to increased yields and improved stabilities. The salts are, moreover, preferably resistant to solution in oil, this property being of especial value in increasing the melting point of the grease.
Examples of suitable salts are: metal benzoate, CsHsC (O) .OM, metal cinnamate,
CsHsCI-I t CHC (O) .OM,
metal salicylate (HO) CsH4C(O) ,OM, metal xylate (CH3) 2C6H3C(0) .OM, and metal vanillate (CI-I30) (HO) CsI-IaC(O) .OM,
and their substituted homologues wherein M represents a metal, such as sodium, potassium, calcium, zinc, and aluminum, but preferably sodium.
The salt present in the composite grease, according to the present invention, is preferably present in concentrations between 0.1% and 6% by weight, although higher concentrations may also be employed. The salt may be formed apart from the step of saponification of the aliphatic material employed for the grease base, and added to the soap, either before or after admixture to mineral oil, and while the soap is heated; it may, however, also be formed in the same operation, as is explained below in the specific examples.
The soda soap may constitute between about 2.5% and 39% of the composite grease. The term soda soap, as used in the present specification and claims, designates sodium salts of carboxylic acids containing at least 10 carbon atoms, as, for examples, salts of higher fatty acids, of naphthenic acids, and of mineral oil sulfonates. While any of the commonly used saponiflable materials may be employed for the production of the soda soap, such as fats and fatty acids, it was found that best results are obtained by employing materials having aliphatic acid residues containing over 20 carbon atoms. Thus, the use of beeswax or degras is preferred over the use of such materials as spermaceti or palm oil. When saponifiable materials consist entirely or mainly of aliphatic acids or of esters of aliphatic acids of between 10 and 20 carbon atoms, it is desirable to add beeswax or degras or a similar material to the extent of at least 40% of the total saponiflables. The use of tallow, spermaceti or similar materials without the addition of materials containing higher aliphatic acids or acid residues often results in the production of a grease having a brittle texture, and may even cause granulation due to soap and oil separation.
The mineral oil constitutes between about 61% and 97.7% of the composite grease. A wide variety of viscous mineral oils may be employed for this purpose. For example, oils having viscosities between about 50 seconds and 250 seconds Say. Univ. at 210 F. may be used. Since, however, the greases, according to the present invention, generally have higher melting points, they must be compounded at elevated temperatures, as, for example, between 500 F. and 620 F., so that because of a fire hazard special precautions must be taken if oils of low flash points, such as those having viscosities less than 100 sec. Say. Univ. at 210 F. are employed. When oils having viscosities above 100 seconds are employed, no special precautions are generally necessary, but it is desirable to carry out the operation in an atmosphere of carbon dioxide or nitrogen when less viscous oils are used.
The grease may, for example, be prepared in the following manner: Approximately 0.5 to 1.0 volumes of the mineral oil and the calculated amount of 45 B. caustic soda are added to the melted saponifiables, the quantity of caustic soda depending upon the saponiilcation numbers of,
the fats, waxes, etc., for any specific formula, and also upon the percentage of the metal salt which is to be employed. The resulting mixture is heated while stirring to a temperature of approximately 250" F. to 325 F., for a period sufflcient to cause saponification, usually between thirty minutes to one hour. The material containing the negative radical of the metallic salt to be employed, such as, for example, benzoic acid, benzaldehyde, or ammonium benzoate, etc., is dissolved in a large body of the oil, and the resulting solution is then added slowly to the soap base while stirring. The balance of the mineral temperatures.
56 ploying the following ingredients:
oil is then added, and the product is heated to a high temperature, for example, 550 F. to 600 F., to destroy any seeds, granules of soap, salt, traces of caustic, etc., which might resist lower Rapid cooling in shallow following the heating is desirable to insure a smooth product.
The invention may be further understood from the following examples:
Example I Two greases, designated below as A and-B, were compounded in the manner described above em Per cent Per cent Beeswax l0. 0 l0. 0 7 acid 2. 0 0
Caustic soda (dry basis) '2. 0 l. 0 8. A. E. 60 motor oil or San Joaquin Valley 86. 0 89. 0
0 at 300 to 500 F. for 24 hours, or storage at 200 to 250 F. for '72 hours, or storage after heating for several months. The eiiect of the presence of the sodium benzoate is apparent from the following table, which compares the properties of the above greases produced under similar @0 61- tions, no sodium benzoate being present in zr'ease B:
Grease A Grease B Unworked penetration 127 00 Worked netration 221 202 Ubbeloh e melting point F.. Above 392 313 Apparent temperature at which product assumes mineral oil fluidity (approximate) F" 650 330 It will be noticed that there is a smaller difference between the worked and unworked penetrations for the grease A, and that this grease has a higher melting point and assumes mineral oil fluidity at considerably higher temperatures than grease B.
- Example I! Two greases, designated as C and D, were similarly compounded, employing degras instead of beeswax, the ingredients being as follows:
- Percent Percent Degras 10. 0 10. 0 Benzoic acid 2. 0 0 Caustic soda (dry basis) 2. 0 l. 3 S. A. E. 60 motor 01] ex San Joaquin Valley. 86.0 88. 7
The grease C was, similar in stability and appearance to the grease A; grease D was, however, slightlygranular and curdled. The properties of the two greases are given below:
Grease O Grease D Unworked penetration-. 104 321 Worked penetration 203 465 Ubbciohde melting point. F Above 392 252 Apparent temperature at which product assumes mineral oil fluidity (approximate) .F. 550 320 acids, hydrocinnamic, naphthoic, alkyl .naphthoic, naphthylacetic and similar monobasic acids, as well as aromatic polybasic acids, like phthalic acid. Moreover, it is not necessary to employ the acid, it being permissible to employ any compound capable of forming a salt with the alkali metal. Thus, ammonium salicylate may be used instead of salicylic acid, ammonia being evolved in the process. Similarly, benzaldehyde may be used for this reaction, sodium benzoate and benzyl alcohol being produced.
The grease compositions of the present invention are useful in solving a large number of lubrication problems in which the high melting points and superior stability of lubricants of the present invention contribute to reduced leakage, more eflicient lubrication, and reduced maintenance costs. A few examples of such applications are: transmission and difierential lubrication, particularly in automobiles, automotive chassis lubrication, universal joint lubrication, roller bearing lubrication, ball bearing lubrication, rocker arm lubrication, particularly in airplanes, journal lubrication in railway equipment, in lumber mills, and in other industrial plants.
The properties of the grease are further apparent from the following tests: 16 grams of grease A of Example I were charged into a ball bearing machine comprising an unloaded ball bearing mounted on a vertical spindle, and surrounded by a grease cup extending several centimeters above the plane of the bearing. The machine was operated for 20 minutes at 4600 R. P. M. without the application of external heat, the temperature rising spontaneously to about 150 F. No pronounced tendency for the lubricant to form fibers or work out of the bearing was noted. At the completion of the test the grease remained unchanged in appearance and structure. There was no evidence of breakdown or of separation of oil and soap.
A similar test was performed for 30 minutes, applying heat to a maximum temperature of 450 F. Similar results were obtained, save that between 240 and 400 F. streamers of grease made their appearance above the plane of the bearing; but adequate lubricant was retained in the bearing in spite of the high speed of operation. Above 400 F. the grease reacted quietly.
I claim as my invention:
1. A soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of an alkali metal salt of an organic carboxylic acid Y containing an aromatic ring to prevent bleeding.
2. A soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of sodium benzoate to prevent bleeding.
3. A soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of sodium salicylate to prevent bleeding.
4. A soda soap grease comprising a viscous mineral oil and a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulfonic acids, said grease containing a minor proportion of sodium cinnamate to prevent bleeding.
5. A soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5 and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids,
naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of an alkali metal salt of an organic carboxylic acid containing an aromatic ring to prevent bleeding.
6. A soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5.and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of sodium benzoate to prevent bleeding.
7. A soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5 and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of sodium salicylate to prevent bleeding.
8. A soda soap grease comprising between 61 and 97.7% of a viscous mineral oil and between 2.5 and 39% of a soda soap of an acid selected from the group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acid, said grease containing between .1 and 6% of sodium cinnamate to prevent bleeding.
9. A soda soap grease comprising a viscous mineral oil and a soda soap of a higher fatty acid, said grease containing a minor proportion of an alkali metal salt of an organic carboxylic acid containing an aromatic ring to prevent bleeding.
10. The grease according to claim 9 in which the soda soap is derived from a saponifiable material selected from the class consisting of beeswax and degras. I
11. A soda soap grease comprising viscous mineral oil and a soda soap of an acid selected from a group consisting of higher fatty acids, naphthenic acids and mineral oil sulphonic acids, at least 40% of said soap consisting of a soda soap of saponifiable material of the type of beeswax, which is rich in fatty acids containing more than 20 carbon atoms, said grease containing a minor proportion of an alkali metal salt of an organic carboxyllc acid containing an aromatic ring to prevent bleeding.
12. The grease according to claim 11 in which the salt is sodium benzoate.
13. The grease according to claim 11 in which the salt is sodium salicylate.
14. The grease according to claim 11 in which the salt is sodium cinnamate. I
VERNON L. RICKE'ITS.
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Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2444970A (en) * 1944-12-30 1948-07-13 Standard Oil Dev Co Grease compositions
US2449312A (en) * 1947-05-07 1948-09-14 Socony Vacuum Oil Co Inc Block greases
US2468098A (en) * 1948-02-18 1949-04-26 Standard Oil Dev Co Grease composition
US2487081A (en) * 1947-11-28 1949-11-08 Standard Oil Co Grease
US2516137A (en) * 1948-10-30 1950-07-25 Standard Oil Dev Co High-temperature lubricating greases
US2516136A (en) * 1948-10-30 1950-07-25 Standard Oil Dev Co Lubricating grease compositions
US2576031A (en) * 1948-10-30 1951-11-20 Standard Oil Dev Co Lubricating grease containing soaps of tall oil
US2576033A (en) * 1949-12-17 1951-11-20 Standard Oil Dev Co Preparing high-temperature lubricating greases
US2586693A (en) * 1949-11-01 1952-02-19 Standard Oil Dev Co Lubricating grease
US2591586A (en) * 1950-09-30 1952-04-01 Standard Oil Dev Co High-temperature lubricating greases
US2614076A (en) * 1949-09-16 1952-10-14 Shell Dev Grease compositions
US2618598A (en) * 1950-02-08 1952-11-18 Standard Oil Dev Co High-temperature lubricating grease
US2623854A (en) * 1950-09-01 1952-12-30 Standard Oil Dev Co Lubricating grease compositions
US2652364A (en) * 1951-12-29 1953-09-15 Shell Dev High-temperature grease compositions
US2690429A (en) * 1952-04-07 1954-09-28 Standard Oil Dev Co Grease compositions containing an aryl oxy alkyl salt as a stabilizer
US2719122A (en) * 1952-01-02 1955-09-27 Exxon Research Engineering Co Complex alkali metal soap-alkaline earth metal salt thickened grease composition
US2801974A (en) * 1952-12-22 1957-08-06 Exxon Research Engineering Co Grease process utilizing the alkali fusion products of cyclic alcohols
US2944970A (en) * 1954-07-12 1960-07-12 Shell Oil Co High temperature grease compositions containing salicylic acid derivatives
US2951808A (en) * 1957-12-31 1960-09-06 Exxon Research Engineering Co Lubricant compositions containing metal salts of aromatic hydroxy carboxylic acids as antioxidants
US2956022A (en) * 1958-03-26 1960-10-11 California Research Corp High extreme pressure grease compositions
US3223632A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of a bicyclo carboxylic acid
US3223627A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of benzoic acid
US3511781A (en) * 1965-04-26 1970-05-12 Chevron Res Complex aluminum greases of enhanced stability
US3514400A (en) * 1967-07-24 1970-05-26 Chevron Res Complex aluminum greases of enhanced stability
EP0366280A1 (en) * 1988-10-26 1990-05-02 Imperial Chemical Industries Plc Grease composition
US20050256013A1 (en) * 2004-05-12 2005-11-17 Davies Kelly J Bar-oil growth retardant

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2444970A (en) * 1944-12-30 1948-07-13 Standard Oil Dev Co Grease compositions
US2449312A (en) * 1947-05-07 1948-09-14 Socony Vacuum Oil Co Inc Block greases
US2487081A (en) * 1947-11-28 1949-11-08 Standard Oil Co Grease
US2468098A (en) * 1948-02-18 1949-04-26 Standard Oil Dev Co Grease composition
US2516137A (en) * 1948-10-30 1950-07-25 Standard Oil Dev Co High-temperature lubricating greases
US2516136A (en) * 1948-10-30 1950-07-25 Standard Oil Dev Co Lubricating grease compositions
US2576031A (en) * 1948-10-30 1951-11-20 Standard Oil Dev Co Lubricating grease containing soaps of tall oil
US2614076A (en) * 1949-09-16 1952-10-14 Shell Dev Grease compositions
US2586693A (en) * 1949-11-01 1952-02-19 Standard Oil Dev Co Lubricating grease
US2576033A (en) * 1949-12-17 1951-11-20 Standard Oil Dev Co Preparing high-temperature lubricating greases
US2618598A (en) * 1950-02-08 1952-11-18 Standard Oil Dev Co High-temperature lubricating grease
US2623854A (en) * 1950-09-01 1952-12-30 Standard Oil Dev Co Lubricating grease compositions
US2591586A (en) * 1950-09-30 1952-04-01 Standard Oil Dev Co High-temperature lubricating greases
US2652364A (en) * 1951-12-29 1953-09-15 Shell Dev High-temperature grease compositions
US2719122A (en) * 1952-01-02 1955-09-27 Exxon Research Engineering Co Complex alkali metal soap-alkaline earth metal salt thickened grease composition
US2690429A (en) * 1952-04-07 1954-09-28 Standard Oil Dev Co Grease compositions containing an aryl oxy alkyl salt as a stabilizer
US2801974A (en) * 1952-12-22 1957-08-06 Exxon Research Engineering Co Grease process utilizing the alkali fusion products of cyclic alcohols
US2944970A (en) * 1954-07-12 1960-07-12 Shell Oil Co High temperature grease compositions containing salicylic acid derivatives
US2951808A (en) * 1957-12-31 1960-09-06 Exxon Research Engineering Co Lubricant compositions containing metal salts of aromatic hydroxy carboxylic acids as antioxidants
US2956022A (en) * 1958-03-26 1960-10-11 California Research Corp High extreme pressure grease compositions
US3223632A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of a bicyclo carboxylic acid
US3223627A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of benzoic acid
US3511781A (en) * 1965-04-26 1970-05-12 Chevron Res Complex aluminum greases of enhanced stability
US3514400A (en) * 1967-07-24 1970-05-26 Chevron Res Complex aluminum greases of enhanced stability
EP0366280A1 (en) * 1988-10-26 1990-05-02 Imperial Chemical Industries Plc Grease composition
US20050256013A1 (en) * 2004-05-12 2005-11-17 Davies Kelly J Bar-oil growth retardant

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