Classifications

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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
  • C10M169/02—Mixtures of base-materials and thickeners
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  • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
  • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
  • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/129—Carboxylix 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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  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/22—Acids obtained from polymerised unsaturated acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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  • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
  • C10M2211/02—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only
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  • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
  • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
  • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
  • C10M2215/064—Di- and triaryl amines
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  • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
  • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
  • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
  • C10M2215/064—Di- and triaryl amines
  • C10M2215/065—Phenyl-Naphthyl amines
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  • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
  • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2217/042—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds between the nitrogen-containing monomer and an aldehyde or ketone
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  • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
  • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2217/043—Mannich bases
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  • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
  • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
  • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
  • C10M2219/108—Phenothiazine
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  • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
  • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
  • C10M2223/04—Phosphate esters
  • C10M2223/041—Triaryl phosphates
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  • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
  • C10M2227/02—Esters of silicic acids
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  • C10M2229/02—Unspecified siloxanes; Silicones
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  • C10M2229/04—Siloxanes with specific structure
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  • C10M2229/04—Siloxanes with specific structure
  • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
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  • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
  • C10N2030/08—Resistance to extreme temperature
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  • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

Definitions

• lubricating compositions suitable for general use throughout the mechanical arts should possess good lubricating properties when operated in either a dry or Wet environment. This latter condition is particularly prevalent in such industrial uses as steel rolling mill applications and the like. Furthermore, the yield of greases prepared from such gelling agents must be as high as possible. The use of resin-coated gelling agents per se has by no means been a panacea for these latter two problems.
• greases exhibiting high water resistance and excellent thermal stability at extremely high temperature both at high yield comprise a lubricating oil gelled to a grease consistency with a colloidally dispersed clay, bearing on its surfaces a resin formed from the co-condensation reaction of melamine and benzoguanamine with an aliphatic aldehyde, the polymer-to-clay weight ratio being from 0.8 to 5.
• the compositions comprise an organosilicone fluid of lubricating oil viscosity gelled to a grease consistency with a colloidally dispersed clay, the surfaces of the clay bearing the abovementioned proportions of melamine-benzoguanamine-aldehyde resin.
• colloidal gelling or thickening agents to be employed are especially selected for use in high-temperature grease compositions due to their relatively inert character at these high operating temperatures. While clays of low base exchange capacity, such as Georgia clay, Attapulgite and the like, may be utilized, it is preferred that a high base exchange clay, such as Wyoming bentonite or hectorite, be employed.
• While the present invention is especially directed to extreme high-temperature lubricating greases, such greases may be employed for normal operating conditions as well. Likewise, superior greases for less severe applications can also be made in accordance with the invention by selection of the lubricating oil base stock.
• most mineral oils are stable up to about 300 F.
• synthetic esters are useful at temperatures up to about 350'- 400 F.
• synthetic lubricating oils of known types such as the phosphorus esters, silicon esters and aliphatic esters formed by esterification of aliphatic dicarboxylic acids with monohydric alcohols. Typical species of these materials include tricresyl phosphate, dioctyl phthalate, bis(2-ethylhexyl)sebacate and the like.
• Lubricants to be employed at temperatures in excess of about 400 F. are those having an inherent high thermal stability including the halocarbons and organo-silicone fluids.
• the halocarbons may be those described in Peterson et al. patent, US. 2,679,479, and include especially the fluorocarbon oils, preferably distilling above about 200 C. at atmospheric pressure.
• the most useful class of lubricants for grease compositions to be utilized at temperatures in excess of about 400 F. include the organosubstituted silicone fluids of lubricating oil viscosity.
• the unreactive, thermally stable silicone fluids which will generally be of the following types:
• Methyl silicone fluids The above types of silicone fluids, in addition to being the most thermally stable are also the most readily available in commercial quantities. Methyl phenyl fluids are particularly preferred because of their still greater thermal stability.
• the viscosity of such polymer or copolymer is, of course, dependent upon the reaction conditions employed in preparing the same, e.g., the polymers of dimethyl silicone vary from thin liquid to viscous liquid to solid resins, depending upon the conditions under which they are prepared. It is the liquid polymers and copolymers having a preferred viscosity exceeding 500 Saybolt seconds at F., which are usually employed in preparing the new compositions.
• thermosetting resins contemplated for use in the compositions of this invention are complex resins, the structure of which is not known, formed by the condensation reaction of melamine and benzoguanamine together with various aldehydes. These amine resins do, however, fall within the class known as aminoplasts as described in the book entitled Fundamentals of Plastics, edited by Richardson and Wilson, Chapters and 6.
• the aldehydes which may be polymerized with the amino compounds include either saturated or unsaturated aldehydes, which may, in turn, be either aliphatic or cyclic. Among those which may be used are formaldehyde, acrolein, furfural, acetaldehyde and crotonaldehyde. For reasons of reactivity as well as thermal stability, it is preferred to use aldehydes containing no more than about six carbon atoms. In the case of aliphatic aldehydes, it is particularly preferred to use only lower alkyl aldehydes, viz. those containing from 1 to 4 carbon atoms per molecule.
• the weight ratio of the resin to the clay be confined to quite narrow limits. Specifically, it has been found that if the resin-to-clay ratio is less than 0.8, the grease may become too fluid upon prolonged exposure to high-temperature operating conditions. A resin-to-clay weight ratio of between 1.0 and 1.5 is especially preferred. Though larger amounts of resin, up to five times the clay weight, may be used, the effectiveness of such heavily coated clay to form a stable grease structure is reduced thereby.
• the ratio of the aldehyde to the melamine and benzoguanamine exerts a profound eifect on the ability of the grease to maintain good lubricating consistency, and that the aldehyde-to-amine ratio must be maintained between quite narrow limits. More particularly, it has been found that satisfactory plasticity of the grease at high temperatures is maintained only if the aldehyde to amine equivalent ratio is maintained between 0.9 and 1.5. At a ratio of 0.9 or less, the grease becomes too dry to lubricate well, and at 1.5 or more the grease becomes crumbly. An aldehyde-to-amine equivalent ratio of 1.0 to 1.4 is therefore preferred.
• Equivalent ratio as used herein refers to the ratio of reactive valences contained in thefractional groups of the two materials being compared.
• the equivalent ratio of one mole of aldehyde to one mole of melamine is 2:6 or 0.3, and to one mole of benzoguanamine is 2:4 or 0.5.
• the ratio of the two amine reactants exerts significant effects on both the water resistance and the yield of the grease composition, which effects are quite unexpected in view of the inability of the corresponding single amine-containing resins to impart these same properties.
• the molar weight ratio of melamine-to-benzoguanamine in the resin with which the clay is coated must be within the limits of from 0.8:1 to 5:1, and preferably from 1:1 to 4:1.
• the process for preparing the greases of the invention since many such procedures are well known in the art. However, all have in common the preparation of an aqueous suspension of the clay prior to forming the resin thereon. Depending upon the physical properties of the particular clay used, the suspension may be a slow-settling slurry or it may be in the form of a more stable hydrogel. Though within this context, the form of the dispersion is not an essential aspect of the invention, the preferred clays happen to form a hydrogel upon being dispersed in water. It is, however, a necessary limitation to the compositions of the invention that they be prepared from an aqueous y i p which. h been aci i ed wit a t g mineral acid.
• the clay be dispersed to yield a hydrogel containing between about 0.25% and about 3% by weight of dry clay, based on the hydrogel before mechanical separation of water therefrom. This percentage is based upon dry weight of de-gangued clay and not upon the dry weight of clay containing naturally occurring contaminants. While the clay is largely dispersed throughout the entire body of the water in which it is incorporated, it is in the form of jelly-like colloidal globules which can be isolated by mechanical separation from a large part of the water to yield a clay hydrogel of substantially increased clay content without shrinking the expanded colloidal structure of the clay.
• mechanical separation any process for the separation of water from the colloid which does not involve a change in physical state such as occurs in normal evaporation methods and the like. Consequently, mechanical separation normally includes filtration techniques and accel erated substitutes therefor, such as centrifuging. This mechanical separation is performed subsequent to the addition to the clay hydrogel of the above-described aminoplast-forming amino compounds.
• the mechanical separation can take place at any desired temperature, room temperature being that preferably employed, although any temperature up to that of the boiling point of water may be utilized.
• the acid must be added in an amount in excess of that required to acidify the surfaces of the clay particles dispersed throughout the hydrogel.
• the amount of acid to acidify the clay i.e., to replace all the basic metals (mostly sodium, potassium, calcium) contained on the clay, will vary depending upon the acid which is used and the base exchange capacity of the clay.
• the amount of acid in the case of hectorite clay to be acidfied with phosphoric acid, the amount of acid must be at least over 7% and preferably about 20% by weight, basis dry clay weight. On the other hand, no more than about 50% and preferably no more than 35% by weight acid should be used.
• phosphoric acid is the preferred strong mineral acid, other mineral acids such as hydrochloric and sulfuric acid may be employed.
• EXAMPLE II Three separate greases were prepared by the process used in Example I, using a diiferent resin in each case.
• a melamine-formaldehyde resin was formed in Sample A
• a benzoguana-mine-formaldehyde was formed in Sample B
• a benzoguanamine-melamine-formaldehyde resin containing an equimolar mixture of the two amines was used in the third sample.
• Each of three greases, which met the requirements for an N.L.G.I. No. 2 grade grease was subjected to ASTM test procedure D 126'4-53T to determine the water washout characteristics of the three greases.
• the mixed amineformaldehyde resin is not a mere mixture of the resin formed from the condensation of benzoguanamine with the aldehyde and of melamine with the aldehyde. To the contrary, it is a much more complex resin since it is formed by the interaction of all three constituents. Because of the complexity of the reaction and the resulting resin structure, which is not fully understood, there is little, if any, predictability of the extrinsic effects of such resins. This lack of predictability is illustrated also by the many critical limitations upon resin composition, as regards the relative proportions of its three constituents, and upon the relative proportions of resin and polymer, all of which were discussed hereinabove. The necessity for these various limitations is illustrated by the following example:
• EXAMPLE III A large number of No. 2 grade greases were prepared in the same manner as Example I in order to examine the effect of compositional variables. Each of the resultant greases was subjected to the ASTM Water Washout test (D 1264-5 3T) and to a high-temperature evaporation and oxidation test.
• the high-temperature test comprised heating a thinfilm sample of the grease on a smooth fiat plate in the presence of air for 300 hours at 450 F., after which the Weight loss of the sample was measured and the texture of the grease was observed.
• the results of these tests were as follows:
• test results of samples 10, 11 and 12 show quite graphically (1) the very great advantage of using the twoamine resin instead of either of the single-amine resins and (2) the profound and unexpected effect of the relative proportion of the amines in the two-amine resin systems.
• the two-amine resin-containing greases exhibited yields comparable to the melamine resin-containing greases and clearly superior to the benzoguanamine resin-containing greases.
• the water washout tests that within the limits of amine molar ratios (melamine-tobenzoguanamine) from about 0.8 to about 4.0, the Water resistance of the greases of the invention were as good as the 'benzoguanamine resin greases and many times superior to the melamine-containing greases. It is especially interesting to note that in increasing the ratio of melamine from 1:1 at least to 3:1, an increase in water resistance was observed.
• a grease composition consisting essentially of a major amount of a lubricating base oil gelled to grease consistency with a colloidally dispersed clay, said clay bearing on the surfaces thereof from 0.8 to 5.0 parts by weight, basis clay, of a resin formed by the co-condensation reaction of the amines melamine and benzoguanamine with an aliphatic aldehyde having up to about 6 carbon atoms, said resin having been formed in the presence of a mineral acid in excess of that required to acidify the surfaces of the clay, the molar ratio of melamine-to-benzoguanamine being from 0.811 to 5 .0: 1, and the equivalent ratio of aldehyde to aliphatic amines being between 09:1 and 1.5:1.
• a grease composition consisting essentially of a major amount of a lubricating base oil gelled to grease consistency with a colloidally dispersed clay, said clay bearing on the surfaces thereof from 1.0 to 5.0 parts by weight, basic clay, of a resin formed by the co-condensation reaction of the amine-melamine and benzoguanamine with an aliphatic aldehyde having up to about 6 carbon atoms, said resin having been formed in the presence of a mineral acid in excess of that required to acidify the surfaces of the clay, the molar ratio of melamine-tobenzoguanamine being from 0.8:1 to 5.0: 1, and the equivalent ratio of aldehyde to aliphatic amines being between 0.921 and 1.5:1.
• a grease composition consisting essentially of a major amount of a lubricating base oil gelled to grease consistency with a colloidally dispersed clay, said clay bearing on the surfaces thereof from 1.0 to 5.0 parts by weight, basis clay, of a resin formed by the co-condensation reaction of the amines melamine and benzoguanamine with an aliphatic aldehyde having up to about 6 carbon atoms, said resin having been formed in the presence of a mineral acid in excess of that required to acidify the surfaces of the clay, the molar ratio of melamine-to-benzoguanamine being from 1.0:1 to 4.021, and the equivalent ratio of aldehyde to aliphatic amines being between 1.0:1 and 1.4: 1.

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• Oil, Petroleum & Natural Gas (AREA)
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• Lubricants (AREA)

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