US2734030A - Mixed soap-complex grease compositions - Google Patents

Mixed soap-complex grease compositions Download PDF

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US2734030A
US2734030A US2734030DA US2734030A US 2734030 A US2734030 A US 2734030A US 2734030D A US2734030D A US 2734030DA US 2734030 A US2734030 A US 2734030A
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    • 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
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    • 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
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/06Well-defined aromatic compounds
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    • 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
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    • 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
    • C10M2207/022Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
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    • 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
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    • 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
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    • 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
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    • 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
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/282Esters of (cyclo)aliphatic oolycarboxylic acids
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/30Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/34Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
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    • 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
    • C10M2209/108Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
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    • 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
    • C10M2209/109Polyethers, i.e. containing di- or higher polyoxyalkylene groups esterified
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/08Thiols; Sulfides; Polysulfides; Mercaptals
    • C10M2219/082Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/02Unspecified siloxanes; Silicones
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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/05Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/04Groups 2 or 12
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    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

Definitions

  • This invention relates to lubricating grease compositions, and particularly to lubricating grease compositions having outstanding high temperature and structure stability properties. More particularly the invention relates to a mixed soap grease containing combined therein a minor amount of a low molecular weight salt in the form of a complex with the mixed soap.
  • these mixed base greases may be improved in structure stability and high temperature performance by complexing with the mixed base soap, a metallic salt of a low molecular weight acid, preferably one having from one to six carbon atoms.
  • a metallic salt of a low molecular weight acid preferably one having from one to six carbon atoms.
  • the incorporation of a salt of a low molecular weight acid in the complex form with the high molecular weight acid soap gives better high temperature performance and increased structure stability.
  • the mixed soap base which serves as the thickening agent for the improved grease compositions of this invention comprises a mixture of the calcium soap of high molecular weight fatty acids and a soap of a metal selected from the class consisting of barium, strontium,
  • the high molecular weight fatty acids operable in preparing the mixed soaps may be selected from the well atoms.
  • the calcium soap must be present in amounts ranging from about 2.5% to about 15.0% by weight, based on the weightof the finished formulation.
  • the amount of the soap of the second metal used is such. that the mol ratio of the c'alcium soap to the second soap is within the range of from 8:1 to 1:8, with a mol ratio within the range of from 8:1 to 3:1 being especially preferred.
  • the amount of the'combined soaps present will depend somewhat upon thedesired'final consistency ofthe'product. Ordinary usage would call for a grease composition according to the instant invention containing from about 5.0% to 30.0% by weight of the combined soap, with a range of from 10.0% to 20.0% being especially preferred.
  • the complexing salt The low molecular weight organic acid salt which is used to form the complex with the mixture of high molecular'weight acid soaps can be derived from any number of organic acids having from one to six carbon
  • the use of acetic or propionic acid is desirable, with acetic being preferred and used in the preferred embodiment.
  • the metal used may be selected from the class consisting of calcium, barium, magnesium, or strontium, with the former being preferred.
  • the salt may be added to the soap mixture in the form of a slurry of the dry salt and oil, in the. form of the dry salt, or it may be prepared in situ.
  • the amount of the salt used will be such as to result in a mol ratio of the total soap to salt of about 0.70 to about 1.2. M01 ratios of greater than 1.2 or less than 0.7 will not produce the results desired.
  • a mol ratio of mixed soaps to the salt of from 0.75 to 1.0 is especially preferred.
  • the lubricating oil base The lubricating oil which is utilized as a dispersant for the soaps in'preparing the greases of invention may be selected from a wide variety of lubricating oils.
  • a mineral lubricating oil preferably of naphthenic origin may be chosen as the base. It should have a viscosity within a range of from about 40 SUS at F. to about 4000 SUS at 100 F.
  • the mineral oil chosen should be that lubricating oil which would be used to furnish proper lubrication if a liquid oil could be used.
  • a mineral lubricating oil such as a conventionally refined distillate
  • a synthetic oil may also be utilized as the dispersing agent.
  • a synthetic lubricant of the ester type is preferred, such as the esters of dibasic acids and long chain alcohols, other well known synthetic lubricants may be used.
  • Complex esters made from dibasic acids, glycols, and alcohols may be used, as may the polymerized glycol esters, glycol ethers, polymerized olefins, alkylated aromatics, polymerized silicones, formals, rnercaptals, and the like.
  • the only requisite for the oil base is that the one chosen be one that will furnish the desired lubrication when utilized as a grease.
  • barium hydroxide is Other additive materials, such as oxidation inhibitors, added in the form of a slurry or as a dry powder to sacolor agents, stringiness or tackiness agents and the like ponify the remainder of the fatty acid.
  • Calcium acetate may also be used in preparing the greases of invention.
  • barium acetate, as the Case y is then added 88 a These agents are ordinarily added after the heating has dry powder or as a water or oil suspension, or if desired been completed and before the grease has cooled coniit may be formed in situ.
  • the soaps are dehydrated and m r ly, heated to above about 350 F.
  • the instant invention relates to base Oil iS then added and the mixture heated to 450 F. superior high temperature lubricating grease composito 480 F. At that temperature the mixture is a homogetions that are prepared by complexing with a mixture neous semi-solid mass. While stirring continuously the of the metallic salts of high molecular weight fatty grease is cooled until the temperature is in the neighboracids, a metallic salt of a low molecular weight acid. d f 50 The Stirring is Then pp and the Specifically, the alkaline earth metals are desired, such grease cooled to room temperature. It is then thoroughly as calcium, barium, strontium, and magnesium.
  • the second and third formulafrom about 5.0 wt. percent to 30.0 wt. percent of the tions were prepared as described in Serial Number total formulation.
  • the low molecular weight salt is 301,194, the copending application mentioned above. added in amounts such that there is present a mol ratio
  • Examples 4 through 9 were prepared in accordance with of total soap to salt of from 0.70 to 1.2, preferably the inventive concept as described in detail above. These from 0.75 to 1.0. It is also essential that the calcium grease samples were submitted to the standard grease in soap be dispersed prior to the dispersion of the barium spection tests including the penetration tests, the detersoap in the mineral oil. mination of the neutralization numbers and the resistance What is claimed is: to boiling water. The data obtained on these 9 greases 1.
  • Soap Type Ca la/Ba Cir Ba (Jo/Ba C's/Ba (Ia/Ba C's/Ba Ca/Ba Oa/Ba High Mol Wt. Soap, M01 Rat-10.. 1 8/ 4/1 8/1 4/1 4/1 4/1 3/1 Percent Saponlf.Material 17 10 10 10 12.5 12.5 10 10 Low M01 Wt.
  • 301,194 has excellent structural stability but its group consisting of calcium, barium, magnesium and strontium, the calcium soap being present in an amount ranging from about 2.5 to 15.0% by weight, based on the weight of the total composition, the moi ratio of said calcium soap to said second soap being about 8:1 to 1:8, the mol ratio of said mixture of soaps to said metal salt being within the range of about 0.70 to 1.2, said complex being formed by first dispersing the calcium soap in the lubricating oil, then dispersing the second soap and said metal salt, and heating the resulting mixture to a transition temperature from about 350 to 480 F. 1
  • said second soap is a barium soap.

Description

United States Patent vllle, N. J., assignors to Esso Research and Engineering Company, a corporation of Delaware No Drawing. Application February 20, 1953,
Serial N0. 338,148
6 Claims. (Cl. 252-39) This invention relates to lubricating grease compositions, and particularly to lubricating grease compositions having outstanding high temperature and structure stability properties. More particularly the invention relates to a mixed soap grease containing combined therein a minor amount of a low molecular weight salt in the form of a complex with the mixed soap.
The preparation of calcium base grease is old in the art and is well described in the patent literature. Such greases are excellent in structure, water resistance, and appearance. However, the high temperature properties of calcium greases are very poor. This is due to the necessity of maintaining a certain amount of water in the grease itself. At temperatures above about 200 F. the water of formulation is driven off and the grease structure breaks down, resulting in separation of the oil.
It has recently been found, and is described in detail in copending application, Serial Number 301,194, filed July 28, 1952, now Patent No. 2,708,659, of which this application is a continuation-in-part, that a calcium base grease having all the advantages of water resistance and characteristic structural stability of the calcium greases, and having, in addition, excellent high temperature properties may be prepared by combining with the calcium soap of the prior art varying amounts of a soap of a metal selected from the group consisting of magnesium, barium, and strontium. Certain processing steps are necessary for the preparation of the greases described in the copending application which are described in detail therein.
It has now been found, and forms the object of this invention, that these mixed base greases may be improved in structure stability and high temperature performance by complexing with the mixed base soap, a metallic salt of a low molecular weight acid, preferably one having from one to six carbon atoms. The incorporation of a salt of a low molecular weight acid in the complex form with the high molecular weight acid soap gives better high temperature performance and increased structure stability.
The mixed soap base The mixed soap base which serves as the thickening agent for the improved grease compositions of this invention comprises a mixture of the calcium soap of high molecular weight fatty acids and a soap of a metal selected from the class consisting of barium, strontium,
and magnesium.
The high molecular weight fatty acids operable in preparing the mixed soaps may be selected from the well atoms.
The calcium soap must be present in amounts ranging from about 2.5% to about 15.0% by weight, based on the weightof the finished formulation. The amount of the soap of the second metal used is such. that the mol ratio of the c'alcium soap to the second soap is within the range of from 8:1 to 1:8, with a mol ratio within the range of from 8:1 to 3:1 being especially preferred. The amount of the'combined soaps present will depend somewhat upon thedesired'final consistency ofthe'product. Ordinary usage would call for a grease composition according to the instant invention containing from about 5.0% to 30.0% by weight of the combined soap, with a range of from 10.0% to 20.0% being especially preferred.
The complexing salt The low molecular weight organic acid salt which is used to form the complex with the mixture of high molecular'weight acid soaps can be derived from any number of organic acids having from one to six carbon The use of acetic or propionic acid is desirable, with acetic being preferred and used in the preferred embodiment. The metal used may be selected from the class consisting of calcium, barium, magnesium, or strontium, with the former being preferred. The salt may be added to the soap mixture in the form of a slurry of the dry salt and oil, in the. form of the dry salt, or it may be prepared in situ. The amount of the salt used will be such as to result in a mol ratio of the total soap to salt of about 0.70 to about 1.2. M01 ratios of greater than 1.2 or less than 0.7 will not produce the results desired. A mol ratio of mixed soaps to the salt of from 0.75 to 1.0 is especially preferred.
The lubricating oil base The lubricating oil which is utilized as a dispersant for the soaps in'preparing the greases of invention may be selected from a wide variety of lubricating oils. A mineral lubricating oil preferably of naphthenic origin may be chosen as the base. It should have a viscosity within a range of from about 40 SUS at F. to about 4000 SUS at 100 F. As in the preparation of most grease compositions, the mineral oil chosen should be that lubricating oil which would be used to furnish proper lubrication if a liquid oil could be used. preferred to use a mineral oil having a viscosity of from about 200 to 1500 SUS at 100 F. to'formulate the greases of the preferred embodiment.
Although a mineral lubricating oil, such as a conventionally refined distillate, is preferred for the preparation of the improved greases of invention, a synthetic oil may also be utilized as the dispersing agent. Although a synthetic lubricant of the ester type is preferred, such as the esters of dibasic acids and long chain alcohols, other well known synthetic lubricants may be used. Complex esters made from dibasic acids, glycols, and alcohols, may be used, as may the polymerized glycol esters, glycol ethers, polymerized olefins, alkylated aromatics, polymerized silicones, formals, rnercaptals, and the like. The only requisite for the oil base is that the one chosen be one that will furnish the desired lubrication when utilized as a grease.
Method .of preparation The same two process limitations described in detail in copending application, ,Serial Number 301,194, pertain to the manufacture of the instant grease formulations; namely, the dispersion of the calcium soap prior to the dispersion of the second soap and heating the total formulation to a temperature of at least 350911 after. dehydration. The exact reasons are not known whythese limitations are critical, but again it is believed that the solu- 3 tion of the calcium soap in the oil aids in the dispersion of the second soap and that above 350 F. there is a phase transition of the soap mixture which produces a new arrangement of molecules that is stable both at low and elevated temperatures. It is also-essential to-raise the mixture to these high temperatures in order to form the complex of the mixture of soaps and the salt, a complex which is believed to be largely responsible for the excellent high temperature and shear stability properties 4 high temperature properties could be improved. This is illustrated by the data of Examples 2 and 3. The data on Examples 4 through 9, prepared in accordance with the instant invention show both excellent high temperature properties and excellent structural stability, at various soap concentrations and complex proportions. It seems clear that the combination ofan alkaline earth metal salt of low molecular weight acids with a mixture of two alkaline earth metal soaps of high molecular weight fatty obtained. to acids produces a grease that is superior to either one The method of manufacture of the greases of this informed from a mere combination of low 'molecular vention may be generally described'as follows. weight salts and a single high molecular weight soap, or p The mixture of high molecular weight soap is prepared a mixture of two high molecular weight oaps alone. first by saponifying a part of the saponifiable material Calcium acetate seems to be the most efiective comwith calcium hydroxide in the presence of one third of plexing agent, with barium acetate being very acceptable. the-total amount of base oil. Then barium hydroxide is Other additive materials, such as oxidation inhibitors, added in the form of a slurry or as a dry powder to sacolor agents, stringiness or tackiness agents and the like ponify the remainder of the fatty acid. Calcium acetate may also be used in preparing the greases of invention. barium acetate, as the Case y is then added 88 a These agents are ordinarily added after the heating has dry powder or as a water or oil suspension, or if desired been completed and before the grease has cooled coniit may be formed in situ. The soaps are dehydrated and m r ly, heated to above about 350 F. The remainder of the To reiterate briefly, the instant invention relates to base Oil iS then added and the mixture heated to 450 F. superior high temperature lubricating grease composito 480 F. At that temperature the mixture is a homogetions that are prepared by complexing with a mixture neous semi-solid mass. While stirring continuously the of the metallic salts of high molecular weight fatty grease is cooled until the temperature is in the neighboracids, a metallic salt of a low molecular weight acid. d f 50 The Stirring is Then pp and the Specifically, the alkaline earth metals are desired, such grease cooled to room temperature. It is then thoroughly as calcium, barium, strontium, and magnesium. Parworked, as by passing through a Morehouse mill or other ticularly desired and contemplated in the preferred emwell known working device. bodiment are the mixtures of the calcium and barium To illustrate the concept of this invention and to point soaps of high molecularv weight fatty acids complexed out the advantages of the new grease formulations over with the calcium salt of a low molecular weight acid those of the prior art, nine grease samples were prepared. having from one to six carbon atoms. Mol ratios of The first preparation was carried out in accordance with from 8:1 to 1:8 of calcium soap to barium soap is the literature and a complex of calcium soap and a calcontemplated, with the 'total soap mixture comprising cium salt was prepared. The second and third formulafrom about 5.0 wt. percent to 30.0 wt. percent of the tions were prepared as described in Serial Number total formulation. The low molecular weight salt is 301,194, the copending application mentioned above. added in amounts such that there is present a mol ratio Examples 4 through 9 were prepared in accordance with of total soap to salt of from 0.70 to 1.2, preferably the inventive concept as described in detail above. These from 0.75 to 1.0. It is also essential that the calcium grease samples were submitted to the standard grease in soap be dispersed prior to the dispersion of the barium spection tests including the penetration tests, the detersoap in the mineral oil. mination of the neutralization numbers and the resistance What is claimed is: to boiling water. The data obtained on these 9 greases 1. A lubricating grease composition having outstandare set out in table form below. ing high temperature properties which comprises a lubri- TABLE Example No 1 2 3 4 5 v 6 7 8 9 High Mo] Wt. Soap Type Ca (la/Ba Cir Ba (Jo/Ba C's/Ba (Ia/Ba C's/Ba Ca/Ba Oa/Ba High Mol Wt. Soap, M01 Rat-10.. 1 8/ 4/1 8/1 4/1 4/1 4/1 4/1 3/1 Percent Saponlf.Material 17 10 10 10 12.5 12.5 10 10 Low M01 Wt. Salt Type Oa-Acc- Ca-Ace- C0-A.ce- Cu-Ace- Ca-Ace- Ba-Ace- Ba-Aceta tate tats tate tats tats tate Percent Low M01 Wt. Salt 3 3 3 2 3 3 M01 tib lz iiiol wt Salt l m l 1.07 1.07 1.07 0.86 0. 57 0.66 0. 86 Dropping Point, 9 F 452 308 282 +520 +520 +520 340 414 3st Penetration in mIIL/IOI Unworkcd' 320 219 286 20s 258 175 175 375 318 Worked (10,000
Worker) 1 430 272 325 368 320 243 280 322 345 Neut. Number, Percent NaOEL 0.12 0. 73 0.13 0. 22 0.28 0. 30 0. 32 0. 47 0. 25 Resistance to boiling water fair excel. excel. excel. excel. excel. excel. excel. excel.
Typical Composition of a Sample (In weight percent):
10% Hydrogenated Fish Oil Acids 3% Calcium acetate 1. 23% Ba(OH)28HzO 1.24% Ca(OH)1 84.48% D10] 2 l Using plate with small holes.
1 Acid treated coastal distillate having a viscosity of 70 S. U. S. at 210 F.
The data of the table above point out the advantage of the greases prepared in accordance with the inventive concept. It will be noted that the calcium-calcium acetate complex grease of the prior art, Example 1, has excellent high temperature properties, but that it fiuidizes after 10,000 strokes with the fine hole worker indicating a lack of structural stability. The Ca/Ba grease of Serial No. 301,194 has excellent structural stability but its group consisting of calcium, barium, magnesium and strontium, the calcium soap being present in an amount ranging from about 2.5 to 15.0% by weight, based on the weight of the total composition, the moi ratio of said calcium soap to said second soap being about 8:1 to 1:8, the mol ratio of said mixture of soaps to said metal salt being within the range of about 0.70 to 1.2, said complex being formed by first dispersing the calcium soap in the lubricating oil, then dispersing the second soap and said metal salt, and heating the resulting mixture to a transition temperature from about 350 to 480 F. 1
2. A lubricating grease composition according to claim 1 wherein the lubricating oil is thickened with from about 10.0 to 20.0% by weight of the complex, based on the weight of the total composition, the mol ratio of said calcium soap to said second soap is between about 8:1 to 3:1, and the mol ratio of said mixture of soaps to said metal is between about 0.75 to 1.0.
3. A lubricating grease composition according to claim 1 wherein said fatty acid contains about 12 to 24 carbon atoms.
- 1 wherein said second soap is a barium soap.
5. A lubricating grease composition according to claim 1 wherein said fatty acid is hydrogenated fish oil acid.
6. A lubricating grease composition according to claim 1 wherein said salt is calcium acetate.
References Cited in the file of this patent UNITED STATES PATENTS Re. 23,032 Zimmer et al. Ian. 25, 1949 2,070,781 Brunstrum et'al Feb. 16, 1937 2,197,263 Carmichael et al. Apr. 16,1940 2,389,523 Leyda Nov. 20, 1945 2,417,429 McLennan Mar. 18, 1947 2,417,433 McLennan Mar. 18, 1947 2,495,651 Butcosk Ian. 24, 1950 2,513,680 Shott et al. July 4, 1950 2,553,423 Shepard May 15, 1951 2,564,561 Carmichael et a1 Aug. 14, 1951 2,583,394 Shott et al. Jan. 22, 1952

Claims (1)

1. A LUBRICATING GREASE COMPOSITION HAVING OUTSTANDING HIGH TEMPERATURE PROPERTIES WHICH COMPRISES A LUBRICATING OIL THICKNESS WITH FROM ABOUT 5.0 TO 30.0% BY WEIGHT, BASED ON THE WEIGHT OF THE TOTAL COMPOSITION, OF A COMPLEX FORMED FROM A MIXTURE OF A CALCIUM SOAP AND A SECOND SOAP SELECTED FROM THE GROUP CONSISTING OF BARIUM, STRONTIUM AND MAGNESIUM SOAPS OF HIGH MOLECULAR WEIGHT FATTY ACIDS AND A METAL SALT OF A LOW MOLECULAR WEIGHT CARBOXYLIC ACID HAVING FROM ONE TO SIX CARBON ATOMS, SAID METAL BEING SELECTED FROM THE GROUP CONSISTING OF CALCIUM, BARIUM, MAGNESIUM AND STRONTIUM, THE CALCIUM SOAP BEING PRESENT IN AN AMOUNT RANGING FROM ABOUT 2.5 TO 15.0% BY WEIGHT, BASED ON THE WEIGHT OF THE TOTAL COMPOSITION, THE MOL RATIO OF SAID CALCIUM SOAP TO SAID SECOND SOAP BEING ABOUT .8:1 TO 1:8, THE MOL RATIO OF SAID MIXTURE OF SOAPS TO SAID METAL SALT BEING WITHIN THE RANGE OF ABOUT 0.70 TO 1.2, SAID COMPLEX BEING FORMED BY FIRST DISPERSING THE CALCIUM SOAP IN THE LUBRICATING OIL, THEN DISPERSING THE SECOND SOAP AND SAID METAL SALT, AND HEATING THE RESULTING MIXTURE TO A TRANSITION TEMPERATURE FROM ABOUT 350* TO 480* F.
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US2856362A (en) * 1956-04-24 1958-10-14 Exxon Research Engineering Co Lubricating compositions
US2918431A (en) * 1956-05-29 1959-12-22 Exxon Research Engineering Co Blended grease compositions
US2973321A (en) * 1957-01-16 1961-02-28 Exxon Research Engineering Co Process of making an improved carboxylic acid salt complex thickened lubricant
DE1233080B (en) * 1960-07-01 1967-01-26 Exxon Research Engineering Co lubricant
DE1233079B (en) * 1953-10-21 1967-01-26 Exxon Research Engineering Co lubricant
US20060090738A1 (en) * 2003-05-23 2006-05-04 Michael Hoffmann Centrifugal oil separator for blow-by gases of an internal combustion engine

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US2197263A (en) * 1939-02-23 1940-04-16 Socony Vacuum Oil Co Inc Grease composition
US2389523A (en) * 1943-11-02 1945-11-20 California Research Corp Barium calcium magnesium stearate grease
US2417429A (en) * 1945-04-16 1947-03-18 Union Oil Co Complex basic soap greases
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US2495651A (en) * 1947-03-20 1950-01-24 Socony Vacuum Oil Co Inc High-temperature ball-bearing grease
US2513680A (en) * 1949-01-18 1950-07-04 Socony Vacuum Oil Co Inc Lime base grease
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USRE23082E (en) * 1949-01-25 Grease compositions
US2583394A (en) * 1952-01-22 Extreme pressure greases
US2070781A (en) * 1935-02-13 1937-02-16 Standard Oil Co Grease
US2197263A (en) * 1939-02-23 1940-04-16 Socony Vacuum Oil Co Inc Grease composition
US2389523A (en) * 1943-11-02 1945-11-20 California Research Corp Barium calcium magnesium stearate grease
US2564561A (en) * 1944-05-20 1951-08-14 Socony Vacuum Oil Co Inc Grease composition
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1233079B (en) * 1953-10-21 1967-01-26 Exxon Research Engineering Co lubricant
US2856362A (en) * 1956-04-24 1958-10-14 Exxon Research Engineering Co Lubricating compositions
US2918431A (en) * 1956-05-29 1959-12-22 Exxon Research Engineering Co Blended grease compositions
US2973321A (en) * 1957-01-16 1961-02-28 Exxon Research Engineering Co Process of making an improved carboxylic acid salt complex thickened lubricant
DE1233080B (en) * 1960-07-01 1967-01-26 Exxon Research Engineering Co lubricant
US20060090738A1 (en) * 2003-05-23 2006-05-04 Michael Hoffmann Centrifugal oil separator for blow-by gases of an internal combustion engine

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