US3620975A - Mixed complex aluminum soap-clay grease composition - Google Patents

Mixed complex aluminum soap-clay grease composition Download PDF

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Publication number
US3620975A
US3620975A US742155A US3620975DA US3620975A US 3620975 A US3620975 A US 3620975A US 742155 A US742155 A US 742155A US 3620975D A US3620975D A US 3620975DA US 3620975 A US3620975 A US 3620975A
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Prior art keywords
grease
clay
aluminum
oil
greases
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US742155A
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Arthur T Polishuk
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Sunoco Inc
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Sun Oil Co
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    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/06—Groups 3 or 13
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • the present invention relates to improved grease compositions. More particularly it relates to grease compositions having exceptional mechanical and thermal properties wherein the improvement arises from a unique mixed-base thickener.
  • Aluminum complex greases are well known and have been established as greases having generally superior properties.
  • Clay-based greases are also well known. Such clay-based greases have excellent resistance to high temperatures. It is substantially impossible to melt such greases, however, the clay-based greases have not received favorable acceptance. It is the general view of those who use greases such as the automotive industry that clay-based greases cause greater wear than soap-based greases because of the abrasive nature of the clay.
  • Another often-voiced criticism of the clay-based greases is their mechanical breakdown in extended use. This occurs in two principal ways First, by breakdown in the grease structure due to shearing forces and secondly, by the separation of oil from the clay thickener. In the latter case, the grease forms a hard cake with essentially no lubricating properties.
  • Aluminum complex soap greases on the other hand, are not as susceptible to these shortcomings and have been widely accepted. in addition, aluminum complex greases have excellent water resistance whereas clays generally are considered to absorb water. A more complete discussion of the various aspects of clay based grease can be found in Manufacture and Application of Lubricating Greases," Boner, C. 1., Reinhold Publishing Corp., New York City, lst Ed. 1954, Ch. 1?, pgs. 677-755.
  • the present invention relates to a complex aluminum soap grease having improved high-temperature and extreme pressure properties as a result of the incorporation therein of a small amount of a clay.
  • the present invention relates to a novel and unique grease composition
  • a novel and unique grease composition comprising mineral lubricating oil thickened to grease consistency with a mixture of complex aluminum soap and a clay.
  • the present invention is a mixed-base grease composition
  • a mixed-base grease composition comprising a major amount of a mineral lubricating oil thickened to grease consistency with a minor amount of a thickening agent comprising a mixture containing l a complex aluminum soap of an aliphatic carboxylic acid containing l2-25 carbon atoms and an aromatic carboxylic acid containing not more than 10 carbon atoms and (2) a cation-modified clay.
  • the present grease compositions contain a major amount, i.e., over 50 percent of oil and a minor amount, i.e., less than 50 percent of a thickener comprising a mixture of a complex aluminum soap and a cation-modified clay.
  • a thickener comprising a mixture of a complex aluminum soap and a cation-modified clay.
  • the total amount of thickener employed can vary depending on the intended use to which the grease is to be put, and generally will be in he range of 1-25 wt. per cent. in any event, the amount of thickener used will be suffi cient to thicken the oil to grease consistency.
  • the amount of cation-modified clay to be used can also be varied depending on he intended use and the desired intensity of a particular set of properties.
  • the improvements noted previously can be obtained by greases wherein the thickener contains from 5 to 95 wt. percent of the cation'modified clay.
  • the grease will contain to 50 wt. percent and more preferably to 50 wt. percent of the cationmodit'ied clay.
  • the grease in addition to the thickener mixture, can contain function materials such as antioxidants, EP additives, stabilizers, additives that improve water washoff, such as, atactic polypropylene, ethylene-vinyl acetate copolymer and the like.
  • function materials such as antioxidants, EP additives, stabilizers, additives that improve water washoff, such as, atactic polypropylene, ethylene-vinyl acetate copolymer and the like.
  • the oil component of the compositions is a mineral lubricating oil.
  • the oil can be paraffinic, naphthenic, or aromatic and could have been prepared by conventional petroleum-refining techniques such as, solvent extraction, sulfuric acid treatment, clay treatment, etc.
  • the oil used will have a viscosity at F. of 505,000 S.U.S. and a VI of 0-130.
  • this thickener system will perform equally well in synthetic oil systems, such as, diesters, polyphenyl ethers, silicone oils, and the like.
  • complex aluminum soaps useful in preparing greases are described in US. Pat. No. 2,768,138 to Hotten and Echols, issued Oct. 23, 1956.
  • a complex aluminum soap is meant, an aluminum soap containing O.8l.5, preferably 1.0-].5, hydroxyl anions per aluminum cation and, at least, two dissimilar carboxylic acid anions.
  • Any individual molecule of the complex aluminum soap consists of one trivalent aluminum cation and three monovalent anions. These anions are selected from the group consisting of hydroxyl anions, relatively oil-soluble carboxylic acid anions, and relatively oil-insoluble carboxylic acid anions.
  • a relatively oil-soluble anion e.g., stearate
  • the aluminum disoap of the anion e.g., aluminum distearate
  • Such anions are preferably obtained from aliphatic carboxylic acids containing 12-25 carbon atoms, examples of such acids being stearic acid, palmitic acid, linoleic acid, tall oil acids, and 12- hydroxystearic acid.
  • a relatively oil-insoluble anion e.g., benzoate
  • the aluminum disoap of the anion e.g., aluminum dibenzoate
  • Such anions are preferably obtained from aromatic carboxylic acids containing not more than 10 carbon atoms, examples of such acids being, benzoic acid, toluic acid and ethylbenzoic acid.
  • the preferred complex aluminum soap is aluminum benzoate stearate.
  • a mixture of relatively oil-soluble anions and relatively oil-insoluble anions can be used. That is, all the relatively oil-soluble anions do not have to be obtained from the same aliphatic carboxylic acid and all the relatively oil-insoluble anions do not have to be obtained from the same aromatic carboxylic acid.
  • One soap molecule may contain two hydroxyl anions and one relatively oil-insoluble anion.
  • Another molecular may contain two relatively oil-insoluble anions and one relatively oil-soluble anion. If mixtures of either relatively oilsoluble anions or relatively oil-insoluble anions are used, further variations between individual soap molecules are possible. In the average soap molecule, however, each of the three types of anions will be present. 7,
  • the ratio of oil-insoluble anions to oil-soluble anions in the complex aluminum soap will usually be in the range of 0.2: l to 5:1, more frequently 0.3:] to 3:], the actual ratio being selected so as to obtain the desired dispersibility of the soap in the oil.
  • the ratio of oil-insoluble anions to oil-soluble anions will generally increase and as the aromaticity decreases this ratio will normally decrease.
  • the ratio of oil-insoluble anions to oilsoluble anions is in the range of 5:1 to 2:0. 1.
  • the aluminum soap can be prepared in the presence of the oil from a substituted cyclic aluminum oxide trimer.
  • the substituted cyclic aluminum oxide trimer has the general formula wherein R is either an alkoxy anion (RO) of an alcohol containing up to 10 carbon atoms or is an acylate anion (RCOO-) of an aliphatic monocarboxylic acid containing 12-22 carbon atoms. These trimers are believed to react with additional carboxylic acids to form the complex aluminum soap.
  • the substituted cyclic aluminum oxide trimers are described in detail in U.S. Pat. No. 2,979,497 to Rinse, issued Apr. 11, 1961. As described in this patent, an aliphatic monocarboxylic acid, an aluminum alkoxide, and water are admixed and held at a temperature of l76248 F. until formation and liberation of alcohol ceases, after which the temperature is raised to and maintained at about 356 F. until further formation and liberation of alcohol ceases.
  • the product is the substituted cyclic aluminum oxide trimer.
  • the substitutions will be either acylate or alkoxy anions depending upon the mol ratios of the reactants used. For example, if the mol ratio of acid to aluminum alkoxide to water is 1:1:1, the product will be the triacylate cyclic aluminum oxide trimer.
  • substitutions on the cyclic aluminum oxide trimers can be a mixture of acylate anions and alkoxy anions, as in the above examples, or can be all acylate anions or all alkoxy anions. Differences in substitutions affect only the amounts of other acids required to complete the reaction. Furthermore, the acylate anions on the trimer do not have to correspond to the particular aliphatic carboxylic acid used. Thus, a trimer containing stearate anions can be reacted with palmitic acid and benzoic acid.
  • the aliphatic anions of the soap are derived from an aliphatic acid per se or from the trimer or from both.
  • the aromatic anions are derived from an aromatic acid and the aluminum cations of the soap are derived from the trimer.
  • the amount of aliphatic acid and aromatic acid to be reacted with the trimer should be such that the ratio of the aliphatic anions, including those present in the trimer, plus the aromatic anions to aluminum cations is in the range of :1 to 3.0: 1, preferably 1.8:1 to 2.6: 1.
  • reaction I 5 mols of carboxylic acid are theoretically required to react with i a mol of trimer containing one aliphatic substitution whereas in reaction 2, 4 moles are theoretically required to react with a mol of trimer containing two aliphatic substitutions.
  • the clay portion of the thickener mixture is a cationmodified clay the preparation of which is shown in U.S. Pat. No. 2,531,427 to Hauser, issued Nov. 28, 1950.
  • the clays which are useful as starting materials are those exhibiting substantial base-exchange properties, and particularly those exhibiting comparatively high base-exchange properties and containing cations capable of more or less easy replacement.
  • the clays particularly contemplated by the specification and the claims include the montmorillonites, viz, sodium, potassium, lithium, and other bentonites, viz, Wyoming and/or California bentonite, magnesium bentonite (sometimes called hectorite, Hector, California) and saponite; also nontronite, attapulgite, illite, zeolites, and fullers earth, particularly those of the Georgia-Florida type.
  • montmorillonites viz, sodium, potassium, lithium, and other bentonites, viz, Wyoming and/or California bentonite, magnesium bentonite (sometimes called hectorite, Hector, California) and saponite; also nontronite, attapulgite, illite, zeolites, and fullers earth, particularly those of the Georgia-Florida type.
  • These clays characterized by an unbalanced atomic structure of unbalanced crystal lattice, are believed to have negative charges which are normally neutralized by inorganic cations. As found
  • the base-exchange capacities of the various clays enumerated run from about 15 to about 100, based upon milliequivalents of exchangeable base per 100 grams of clay.
  • montmorillonites have comparatively high base-exchange capacities, viz, -100. Attapulgite and illite have substantial base-exchange capacities, viz, 25-35 and 15-50, respectively. Generally, the clays of higher base-exchange capacities, i.e., of at least 25 are particularly useful where high exchange of an organic base for the cation of the clay is desired.
  • a clay of the character described and exhibiting substantial base-exchange capacity is reacted with an organic compound, more particularly one hereinafter generally defined and referred to as an onium compound, by substitution of the clay cation of the organic compound, which cation is of a class hereinafter referred to as an onium" base.
  • An onium compound is defined as a group of organic compounds of the type:
  • RXl-ly which are isologs of ammonium and contain the element X in its highest positive valency.
  • the onium base radical exchanged for the inorganic radicals of the clay is hydrophobic as distinguished from hydrophilic, so as to convert the clay from a hydrophilic to an organophilic condition.
  • a preferred type of onium compound is an organic amine.
  • These compounds may include salts of aliphatic, cyclic, aromatic, and heterocyclic amines, primary, secondary, and tertiary amines and polyamines, also quaternary ammonium compounds. lt has been found that a base with a molecular area of about square angstrom units, for example, a primary amine with a straight aliphatic chain of 10 carbons atoms, e.g., decyl amine, will substantially fulfill the requirements of covering the clay surface.
  • Other types of amines may be used also, e.g., tertiary amines such as, lauryl dimethyl amine.
  • the particular type of clay to be used can be varied depending on the intended use. The montmorillonites, bentonite and hectorite are particularly useful, more particularly the bentonites because of their exceptional gellation properties.
  • the novel greases of the present invention can be prepared by preparing a complex aluminum grease and a cation-modified clay grease separately then blending the finished greases in the desired proportions.
  • the greases of the invention can be prepared by blending a complex aluminum grease and a cation-modified clay grease, or the complex aluminum, cation-modified clay grease can be prepared in situ in the same batch of base oil, that is, by forming a mixed base grease directly.
  • the preparation of aluminum complex and modified clay greases generally is well known in the art, for example, the Hotten and Echols patent previously mentioned in regard to complex aluminum greases and U.S. Pat. No. 2,531,440 to Jordan, issued Nov. 28, 1950, in regard to cation-modified clay greases, and needs no discussion here, however, a brief description of the process used for producing the aluminum complex grease from the substituted cyclic aluminum trimer is given.
  • Such equipment normally includes a grease kettle equipped with heating facilities and an agitator.
  • Conventional agitators are usually of the paddle type and turn at 15-75 r.p.m. being designed merely to keep the contents of the kettle in motion without creating any areas of very vigorous agitation.
  • the aliphatic acid is first mixed with a portion of the base lubricating oil and the mixture is heated to a temperature in the range of l80250 F., preferably l90-220 F., at which temperature the trimer is mixed in.
  • the trimer aliphatic acid-base oil mixture is held at this temperature for a period of 5 minutes to 5 hours, preferably 10 minutes to 2 hours.
  • the reaction time should be adjusted to the temperature so that shorter reaction times are employed at higher temperatures.
  • the aliphatic acid can be mixed with the oil and trimer at a low temperature and the entire mixture then heated up, or the oil can be heated up and both the trimer and acid then mixed in.
  • the order in which the three ingredients are mixed is not critical.
  • the cation-modified clay can be added at this point, however, it is preferably added just prior to the milling of the grease.
  • the aromatic acid is mixed in.
  • the aromatic acid should be mixed with the remainder of the base oil and added in liquid phase form and with agitation to the trimer-aliphatic acid phase.
  • Conventional grease kettle agitators, described hereinbefore, will provide sufficient agitation for the proper incorporation of the aromatic acid.
  • the temperature of the mix should be held within the range of l80-250 F while the aromatic acid is being added.
  • the aromatic acid can be added at the same time as the aliphatic acid.
  • the mass should be raised to a temperature in the range of 400-460 F., preferably 410430 F.
  • the time required to reach this temperature is preferably in the range of 1-5 hours, although higher or lower heating periods can also be used.
  • the mass should be maintained at 400-460 F. for a period of 10 minutes to 6 hours, preferably minutes to 2 hours.
  • the mass After the mass is held at 400-460 F. for the prescribed period, it should be cooled to a temperature in the range of l00-25O F. at which temperature it should be milled. In order to prevent the mass from becoming gelatinous during this cooling step, the cooling should be relatively slow, i.e., it should occur over a period of at least 1 hour. Cooling periods longer than 1 hour can be utilized, but are no t necessary.
  • the mass Upon cooling to l00-250 F., the mass should be milled. Milling is necessary in order to obtain a grease of uniform composition and which has a smooth and uniform texture.
  • additives such as, oxidation inhibitors, extreme pressure agents, etc. are to be incorporated into the grease, they are preferably added just prior to the milling step, although an antioxidant can be added at the begirining to prevent oxidation of the oil during the heating cycle.
  • the cation-modified clay can also be added at this point.
  • a cationmodified grease is prepared and blended with aluminum complex grease after milling. The following examples are present to illustrate the invention, and at least one of its embodiments.
  • the oil employed in the examples was a naphthenic oil having the following properties:
  • clay portion of the thickener contributes its high-temperature properties to the aluminum complex soap grease with no loss in the long-range performance of the aluminum complex soap grease.
  • An added benefit is improvement of the initial properties of the aluminum complex soap grease by the bentonite as can be seen from table ll].
  • a mixed-base grease composition comprising a major amount of a mineral lubricating oil thickened to grease consistency with synergistic proportions of i) an aluminum complex soap of stearic acid and benzoic acid and (2) an onium base cation-modified bentonite clay.
  • a mixed-base grease according to claim 1 where the cation-modified clay is 25 to 50 wt. percent of the thickeners.

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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)
US742155A 1968-07-03 1968-07-03 Mixed complex aluminum soap-clay grease composition Expired - Lifetime US3620975A (en)

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DE (1) DE1927373C3 (enrdf_load_stackoverflow)
FR (1) FR2012238B1 (enrdf_load_stackoverflow)
GB (1) GB1259379A (enrdf_load_stackoverflow)
SE (1) SE343877B (enrdf_load_stackoverflow)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4132658A (en) * 1978-03-27 1979-01-02 Texaco Inc. Process for manufacturing aluminum complex soap thickened grease
WO2001066675A3 (de) * 2000-03-10 2002-06-27 Sasol Germany Gmbh Verdickungsmittel-komponente und aluminiumkomplex-schmierfett
US20070129267A1 (en) * 2005-12-05 2007-06-07 Mishra Gopal S Lubricating grease composition
CN109705960A (zh) * 2019-01-25 2019-05-03 清华大学 润滑剂及其制备方法，以及降低流体粘度的方法
CN111996064A (zh) * 2020-09-23 2020-11-27 上海虎头化工有限公司 一种超高温润滑脂及其制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2968670B1 (fr) 2010-12-13 2013-01-04 Total Raffinage Marketing Composition de graisse

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2768138A (en) * 1952-10-18 1956-10-23 California Research Corp Complex basic aluminum soap greases
US2875152A (en) * 1955-12-20 1959-02-24 Shell Dev Process for the preparation of greases gelled with non-soap gelling agents
US3106532A (en) * 1960-05-12 1963-10-08 Lab Riuniti Studi E Ricerche S Process for preparing improved compositions of lubricating greases

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL73983C (nl) * 1949-12-27 1954-01-15 Bataafsche Petroleum Werkwijze voor het polymeriseren van onverzadigde verbindingen, in water geëmulgeerd.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2768138A (en) * 1952-10-18 1956-10-23 California Research Corp Complex basic aluminum soap greases
US2875152A (en) * 1955-12-20 1959-02-24 Shell Dev Process for the preparation of greases gelled with non-soap gelling agents
US3106532A (en) * 1960-05-12 1963-10-08 Lab Riuniti Studi E Ricerche S Process for preparing improved compositions of lubricating greases

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4132658A (en) * 1978-03-27 1979-01-02 Texaco Inc. Process for manufacturing aluminum complex soap thickened grease
WO2001066675A3 (de) * 2000-03-10 2002-06-27 Sasol Germany Gmbh Verdickungsmittel-komponente und aluminiumkomplex-schmierfett
US20040097381A1 (en) * 2000-03-10 2004-05-20 Peter Finmans Thickener component and lubricating grease containing an aluminium complex
US20060019842A1 (en) * 2000-03-10 2006-01-26 Peter Finmans Aluminum complex grease
US20070129267A1 (en) * 2005-12-05 2007-06-07 Mishra Gopal S Lubricating grease composition
US7767634B2 (en) 2005-12-05 2010-08-03 Indian Oil Corporation Limited Lubricating grease composition
CN109705960A (zh) * 2019-01-25 2019-05-03 清华大学 润滑剂及其制备方法，以及降低流体粘度的方法
CN111996064A (zh) * 2020-09-23 2020-11-27 上海虎头化工有限公司 一种超高温润滑脂及其制备方法

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GB1259379A (enrdf_load_stackoverflow) 1972-01-05
SE343877B (enrdf_load_stackoverflow) 1972-03-20
FR2012238B1 (enrdf_load_stackoverflow) 1974-08-02
DE1927373A1 (de) 1970-08-27
FR2012238A1 (enrdf_load_stackoverflow) 1970-03-13
DE1927373C3 (de) 1978-05-03

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