Triurea grease compositions

BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to grease compositions using novel triurea compounds which are excellent in oil separation, shear stability and oxidation stability at a high temperature and are noticeably stable in the structure of a thickening agent under severe conditions of oxidation or high temperature and the like.
2. Description of the Prior Art
Presently most broadly used greases are ones using a metal soap as a thickening agent and among them, lithium soap grease has been generally numerously used. However, greases having higher quality and longer durable life have been demanded as the lubricating conditions become more severe owing to the progress of machines and novel thickening agents having excellent thermal resistance and long durable life at a high temperature have been gradually developed.
Among the thus developed greases, urea greases are non-soap ones and contain an ashless thickening agent and therefore these greases are one of representable high temperature greases. In general, these greases are high in dropping point and are relatively stable in the structure of the thickening agent at a high temperature and contain no metallic atom which promotes the oxidation deterioration in the molecule of the thickening agent, so that the oxidation stability is generally high.
Urea compounds of the thickening agent may be produced by reacting an isocyanate with an amine in a solvent or a base oil but the urea compounds of the reaction products include a large number of urea compounds depending upon the number of urea bond ##STR2## ureilene radical), and the kind or number of radicals (hydrocarbon radicals, etc.) between the urea bonds and terminal radical of the compound, and there is a great difference in the grease property.
The most typical prior patents already reported comprise diurea grease by E. A. Swakon et al (U.S. Pat. No. 2,710,839, U.S. Pat. No. 2,710,840, U.S. Pat. No. 2,710,841) and tetraurea grease by J. L. Dreher et al (U.S. Pat. Nos. 3,242,210, 3,243,372) and the other many patents intend to develop these base patents and improve the grease properties.
However, in general the diurea greases have defects that at a high temperature the consistency softens and the oil separation is high and the tetraurea greases when exposing to a high temperature for a long period of time, readily cause the hardening of consistency. Furthermore, in the prior triurea greases (Japanese Patent No. 932,322), the consistency softens at a high temperature and in symmetrical triazine tetraurea greases (U.S. Pat. Nos. 4,026,890 and 4,113,640), the production of the thickening agent is troublesome and a long time is necessary for obtaining the final grease product.
SUMMARY OF THE INVENTION
The inventors have made studies for obviating the above described defects of the prior arts and found that triurea compounds in which a triazine radical is introduced between urea bonds, have very excellent properties as a thickening agent of a grease and that a method for producing the grease is relatively easy.
That is, asymmetrical triazine triurea greases according to the present invention have a high dropping point, are excellent in the oil separation, shear stability and oxidation stability at a high temperature and are considerably small in the variation of the grease condition after oxidation at a high temperature and when the heating and cooling are repeated, the initial consistency is substantially maintained and thus the high temperature properties are very excellent.
The greases according to the present invention can use a wide variety of lubricating oils of mineral oil and synthetic oils as the base oil and any lubricaing oils in which the viscosity is within the range of the usually used lubricating oils, can be used.
A grease composition of the present invention consists essentially of a major amount of a lubricating base oil and 2-30% by weight, preferably 4-25% by weight of a thickening agent of a triurea compound having the general formula ##STR3## wherein R.sub.1 is a monovalent aliphatic hydrocarbon radical having 12-24 carbon atoms, R.sub.2 is a divalent triazine derivative radical, R.sub.3 is a divalent aromatic hydrocarbon radical having 6-15 carbon atoms or the derivative radical thereof, and R.sub.4 is at least one of monovalent aliphatic hydrocarbon radicals having 2-24 carbon atoms, derivative radicals thereof, monovalent aromatic hydrocarbon radicals having 6-10 carbon atoms and derivative radicals thereof.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As the monovalent aliphatic hydrocarbon radicals (R.sub.1) having 12-24 carbon atoms, mention may be made of the aliphatic hydrocarbon radicals having a straight chain structure, such as dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, nonadecyl, eicosyl, heneicosyl, docosyl, tricosyl, tetracosyl radicals, and hexadecyl, octadecyl and eicosyl radicals are particularly preferable.
As the divalent triazine derivative radicals (R.sub.2), mention may be made of ##STR4## wherein R is a monovalent aliphatic hydrocarbon radical having 12-24 carbon atoms and -C.sub.6 H.sub.5 is a phenyl radical, and the particularly preferable radicals are ##STR5##
As the divalent aromatic hydrocarbon radicals (R.sub.3) having 6-15 carbon atoms or the derivative radicals thereof mention may be made of ##STR6##
As the aliphatic hydrocarbon radicals (R.sub.4) having 2-24 carbon atoms, mention may be made of saturated or unsaturated aliphatic hydrocarbon radicals such as octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, octadecynyl, nonadecyl, eicosyl, heneicosyl, docosyl, tricosyl and tetracosyl radicals and the particularly preferable ones are hexadecyl, octadecyl and octadecynyl radicals. The derivative radicals thereof include monoethanolamine, isorpopanolamine, palmitic acid amide, stearic acid amide, etc.
As the monovalent hydrocarbon radicals (R.sub.4) having 6-10 carbon atoms, mention may be made of ##STR7##
As the derivative radicals (R.sub.4) thereof, mention may be made of ##STR8## wherein X is a halogen atom such as fluorine, chlorine and bromine.
When the carbon number of R.sub.1 in the above described general formula is less than 11, the oleophilic property lowers, while when said number is more than 25, the solubility lowers and the reactivity becomes poor, so that these cases are not acceptable.
R.sub.3 is an aromatic hydrocarbon radical and therefore the carbon number must be 6 or more and when said number exceeds 15, both the solubility and the reactivity lower, so that such a case is not applicable.
When the carbon number of R.sub.4 is less than 2, that is 1, such an amine is gaseous and the control of the reaction is difficult, while when said number is more than 25, the solubility lowers and the reactivity also lowers, so that both the cases are not acceptable. When R.sub.4 is an aromatic hydrocarbon radical, the carbon number must not be less than 6 and when said number exceeds 10, both the solubility and the reactivity lower.
Then, explanation will be made with respect to the method for producing novel triurea compounds to be used as the thickening agent in the present invention. The triurea compounds are the reaction product of an N-aliphatic hydrocarbon radical substituted ureido-triazine derivative, one or more primary amines and a diisocyanate, which is shown by the following chemical reaction formula. ##STR9##
In the above described chemical reaction, the primary amine may be a combination of two or more amines as well as a single amine. When the primary amine is used in a single amine, the grease obtained from the triurea compound formed from such an amine may have an individual property of a merit and a demerit, while when two or more different amines are used in a combination, the obtained grease can develop balanced properties of these amines, so that the use of two or more amines is preferable.
The above described N-aliphatic hydrocarbon radical substituted ureido-triazine derivatives are produced by reacting a triazine derivative having two or more amino radicals with an alkyl isocyanate having 12-24 carbon atoms and this reaction is shown by the following general formula ##STR10##
This reaction may be carried out in an equimolar ratio of an alkyl isocyanate and a triazine derivative and as an auxiliary solvent, it is preferable to use a polar organic solvent, such as dimethylformamide, dioxane, dimethylsulfoxide, etc. The reaction temperature is generally 80.degree.-200.degree. C., preferably 100.degree.-160.degree. C. and the reaction is carried out while stirring for 1-5 hours. The reaction product precipitates in the solvent, so that after completing the reaction, the reaction mass is cooled to room temperature and then filtered and the reaction product is dried to obtain N-aliphatic hydrocarbon radical substituted ureido-triazine.
The production method of a grease is as follows.
N-aliphatic hydrocarbon radical substituted ureido-triazine derivative and one or more primary amines are mixed in an equimolar ratio in a lubricating base oil and heated and dissolved and then a diisocyanate (a solution in the lubricating base oil) is gradually added in an equimolar ratio thereto while vigorously stirring. Then, the reaction product is heated to a given temperature (150.degree.-220.degree. C.) while thoroughly stirring, after which the reaction mixture is cooled to room temperature and milled to obtain the product.
In the method of the above mentioned U.S. Pat. Nos. 4,026,890 and 4,113,640, wherein this reaction is not performed in a lubricating base oil, but in a volatilizing organic solvent, troublesome operations such as removal of a solvent, grinding of the reaction product and incorporating into the lubricating base oil, are necessary and this method has a drawback that a long time is required for the preparation. Accordingly, the present invention wherein the preparation is performed in the lubricating base oil is more advantageous than these prior arts.
The thus prepared grease compositions may be added with additives such as extreme pressure additives, oxidation inhibitors, oil improvers, anticorrosion additives, viscosity index improvers and the like without damaging the properties in order to improve the grease performances.
The content of the triurea compounds is preferred to be 2-30% by weight, preferably 4-25% by weight. When the amount of the triurea compounds are less than 2% by weight, the thickening activity is lower, while when said amount exceeds 30% by weight, the grease becomes too hard and a satisfactory lubricating effect cannot be attained and such an amount is disadvantageous in view of economy.
The thus prepared greases show superior properties to the other prior commercially available greases as explained in the following examples.

The following examples are given for the purpose of illustration of this invention and are not intended as limitations thereof.
EXAMPLES 1-30
87.5 g of 2-octadecylureido-4-octadecylamino-1,3,5-triazine, 35.0 of octadecylamine and 445.0 g of paraffin refined mineral oil (Kinematic viscosity @100.degree. C., 10.48 cst, viscosity index 99) were charged in a reaction vessel and uniformly mixed and dissolved by heating up to about 80.degree. C. Separately, 32.5 g of an equimolar ratio of diphenylmethane-4,4'-diisocyanate has been uniformly dissolved in 400 g of the same paraffin refined mineral oil as described above by heating at about 80.degree. C. and this solution was gradually added to the above described mixture while vigorously stirring. The resulting mixture subsequently was heated up to 185.degree. C. while vigorously stirring. Then, the reaction mixture was cooled to room temperature and roll-finished to obtain a smooth grease.
The properties of the obtained greases are shown in the following Table 2.
In Examples 2-30, the grease compositions were prepared in the same manner as described in Example 1 except for varying the used starting material and the highest treating temperatures for the preparation as shown in the following Table 1.
TABLE 1__________________________________________________________________________ HighestTriazine treatingderivatives Primary amines Diisocyanates Base oils temperatureExample Kind g Kind g Kind g Kind g (.degree.C.)__________________________________________________________________________2 DSM* 105.2 Octadecylamine 20.2 MDI**** 37.5 Paraffin mineral oil 829.1 185 p-toluidine 8.0 (Kinematic viscosity @ 100.degree. C., 10.48 cst)3 MCG** 63.2 Octadecylamine 20.2 MDI 37.5 Paraffin mineral oil 857.9 160 Stearic acid amide 21.2 (Kinematic viscosity @ 100.degree. C., 13.59 cst)4 DSM 98.1 Hexadecylamine 16.9 MDI 35.0 Pentaerythritol 841.4 200 p-anisidine 8.6 tetracaprate (Kinematic viscosity @ 98.9.degree. C., 7.34 cst)5 ATT*** 101.0 Oleylamine 20.0 TODI***** 39.6 Methylphenyl 831.4 220 p-toluidine 8.0 polysiloxane (Kinematic viscosity @ 25.degree. C., 400 cst)6 MCG 63.2 Octadecylamine 20.2 TODI 39.6 Paraffin mineral oil 867.5 200 p-chloroaniline 9.5 (Kinematic viscosity @ 100.degree. C., 13.59 cst)7 MCG 58.2 Octadecylamine 37.2 MDI 34.6 Paraffin mineral oil 870.0 170 (Kinematic viscosity @ 100.degree. C., 13.59 cst)8 DSM 80.4 Octadecylamine 30.9 MDI 28.7 Paraffin mineral oil 860.0 170 (Kinematic viscosity @ 100.degree. C., 13.59 cst)9 DSM 99.4 p-toluidine 15.2 MDI 35.4 Paraffin mineral oil 850.0 170 (Kinematic viscosity @ 100.degree. C., 32.89 cst)10 ATT 95.4 Hexadecylamine 34.2 MDI 35.4 Paraffin mineral oil 835.0 185 (Kinematic viscosity @ 100.degree. C., 32.89 cst)11 MCG 75.0 Stearic acid amide 50.4 MDI 44.6 Paraffin mineral oil 830.0 200 (Kinematic viscosity @ 100.degree. C., 32.89 cst)12 MCG 79.5 p-anisidine 23.2 MDI 47.2 Paraffin mineral oil 850.1 170 (Kinematic viscosity @ 100.degree. C., 32.89 cst)13 MCG 61.8 Octadecylamine 39.5 TODI 38.7 Pentaerythritol 860.0 200 tetracaprate (Kinematic viscosity @ 98.9.degree. C., 7.34 cst)14 ATT 84.9 Aniline 11.7 TODI 33.3 Pentaerythritol 870.1 200 tetracaprate (Kinematic viscosity @ 98.9.degree. C., 7.34 cst)15 ATT 70.0 Octadecylamine 19.6 TODI 27.5 Paraffin mineral oil 880.0 160 Aniline 2.9 (Kinematic viscosity @ 100.degree. C., 10.48 cst)16 DSM 95.3 Oleylamine 21.8 TODI 35.9 Paraffin mineral oil 840.0 185 p-chloroaniline 7.0 (Kinematic viscosity @ 100.degree. C., 13.59 cst)17 DSM 88.7 Hexadecylamine 24.4 TODI 33.4 Methylphenyl 850.0 220 p-phenetydine 3.5 polysiloxane (Kinematic viscosity @ 25.degree. C., 400 cst)18 DSM 106.3 Octadecylamine 12.2 TODI 40.0 Paraffin mineral oil 835.0 170 Monoethanolamine 6.5 (Kinematic viscosity @ 100.degree. C., 32.89 cst)19 ATT 68.5 Octadecylamine 21.9 TODI 26.9 Paraffin mineral oil 879.9 200 p-phenetydine 2.8 (Kinematic viscosity @ 100.degree. C., 32.89 cst)20 MCG 77.1 Palmitic acid amide 32.7 TODI 48.4 Paraffin mineral oil 835.1 185 p-anisidine 6.7 (Kinematic viscosity @ 100.degree. C., 13.59 cst)21 MCG 58.3 Octadecylamine 18.6 MDI 34.6 Methylphenyl 880.0 200 p-anisidine 8.5 polysiloxane (Kinematic viscosity @ 25.degree. C., 400 cst)22 ATT 98.8 Stearic acid amide 29.1 MDI 36.7 Paraffin mineral oil 830.0 185 p-anisidine 5.4 (Kinematic viscosity @ 100.degree. C., 10.48 cst)23 ATT 91.2 Octadecylamine 7.3 MDI 33.9 Paraffin mineral oil 840.0 185 Palmitic acid amide 27.6 (Kinematic viscosity @ 100.degree. C., 32.89 cst)24 DSM 96.8 Octadecylamine 7.4 MDI 34.5 Paraffin mineral oil 830.1 170 Stearic acid amide 31.2 (Kinematic viscosity @ 100.degree. C., 32.89 cst)25 DSM 78.4 Hexadecylamine 13.5 MDI 28.0 Paraffin mineral oil 874.9 170 Aniline 5.2 (Kinematic viscosity @ 100.degree. C., 32.89 cst)26 DSM 77.7 Octadecylamine 14.9 MDI 27.7 Paraffin mineral oil 870.0 170 Palmitic acid amide 7.1 (Kinematic viscosity Aniline 2.6 @ 100.degree. C., 32.89 cst)27 MCG 60.3 Octadecylamine 19.3 MDI 35.8 Paraffin mineral oil 870.1 180 Stearic acid amide 10.1 (Kinematic viscosity p-anisidine 4.4 @ 100.degree. C., 32.89 cst)28 MCG 75.8 Octadecylamine 19.4 MDI 45.0 Paraffin mineral oil 849.9 170 Isopropanolamine 2.7 (Kinematic viscosity p-toluidine 3.9 @ 100.degree. C., 32.89 cst) Aniline 3.329 MCG 75.1 Hexadecylamine 25.8 MDI 44.6 Paraffin mineral oil 840.0 185 Stearic acid amide 10.1 (Kinematic viscosity p-phenetidine 2.5 @ 100.degree. C., 32.89 cst) p-toluidine 1.930 ATT 84.3 Octadecylamine 13.5 MDI 31.3 Paraffin mineral oil 859.9 200 Stearic acid amide 7.1 (Kinematic viscosity Monoethanolamine 2.3 @ 100.degree. C., 32.89 cst) p-chloroaniline 1.6__________________________________________________________________________ Note:- *DSM: **MCG: ***ATT: ****MDI: *****TODI: 3,8bitolylene-4,4diisocyanate-
The properties of the greases obtained in the above described examples are shown in the following Table 2. The same test was performed with respect to the commercially available urea greases (Comparative Example 1: a commercially available diurea grease, Comparative Example 2: a commercially available tetraurea grease, Comparative Example 3: a commercially available triurea grease) and the properties of these greases are shown in the following Table 2. Test methods:
1. Worked penetration: Following to ASTM D217
2. Dropping point: Following to ASTM D566
3. Oil separation: Following to FTM 791 B-321.2
4. Oxidation stability:
(1) Following to ASTM D942, the test was performed at 150.degree. C. for 200 hours.
(2) The worked penetration of the grease after the test was measured by means of 1/4-scale cone following to ASTM D1403, reference 1.
(3) Dropping point of the grease after the test was followed to ASTM D566.
5. Heating-cooling cycle test:
A sample was charged and filled in a pot for measuring 1/2 scale cone penetration and heating in an air bath kept at a constant temperature of 150.degree. C. and 180.degree. C. for 20 hours and then taken out and cooled in air for 4 hours.
Unworked penetration was measured by means of 1/2 scale cone following to ASTM D1403 reference 1. This operation was conducted in 4 cycles.
6. Roll stability:
This test was conducted following to ASTM D1831 at 100.degree. C. for 24 hours and at 150.degree. C. for 24 hours.
TABLE 2__________________________________________________________________________ Example Example Example Example Example Example ExampleTest items 1 2 3 4 5 6 7__________________________________________________________________________Worked penetration 274 285 283 279 277 280 285Dropping point (.degree.C.) 258 275 274 268 269 265 257Oil separation100.degree. C., 24 hr (%) 1.4 0.9 0.6 1.0 0.8 1.2 0.8150.degree. C., 24 hr (%) 1.0 0.7 1.3 1.2 0.7 1.0 0.4Oxidation stability 2.00 2.25 2.15 2.15 2.05 2.20 1.95150.degree. C., 200 hr (kgf/cm.sup.2)Form of grease after test grease- grease- grease- grease- grease- grease- grease- like like like like like like likeWorked penetration of grease after test 276 290 294 291 300 294 298Dropping point of grease after test (.degree.C.) 249 268 273 265 260 257 252Heating-cooling cycle testUnworked penetration after cycle 1 cycle 239 258 246 251 236 254 251of heating at 150.degree. C. for 20 hours 2 cycle 240 253 249 244 240 246 250and cooling by leaving in air 3 cycle 235 259 251 238 234 241 246for 4 hours 4 cycle 235 242 260 239 231 239 246Unworked penetration after cycle 1 cycle 245 263 251 250 253 252 255of heating at 180.degree. C. for 20 hours 2 cycle 263 269 272 263 250 260 261and cooling by leaving in air 3 cycle 275 271 289 274 259 273 270for 4 hours 4 cycle 280 285 294 289 267 287 284Roll stability100.degree. C., 24 hr 290 298 291 296 291 290 315150.degree. C., 24 hr 286 297 293 300 291 302 310__________________________________________________________________________ Example Example Example Example Example Example ExampleTest items 8 9 10 11 12 13 14__________________________________________________________________________Worked penetration 269 280 281 274 290 284 278Dropping point (.degree.C.) 263 262 270 268 263 274 280Oil separation100.degree. C., 24 hr (%) 1.2 1.5 0.7 1.1 0.9 0.9 1.4150.degree. C., 24 hr (%) 0.8 0.9 0.4 0.6 0.6 0.3 1.0Oxidation stability 2.10 2.35 2.25 2.25 2.20 2.00 2.20150.degree. C., 200 hr (kgf/cm.sup.2)Form of grease after test grease- grease- grease- grease- grease- grease- grease- like like like like like like likeWorked penetration of grease after test 276 302 300 285 292 284 287Dropping point of grease after test (.degree.C.) 251 253 268 261 259 268 273Heating-cooling cycle testUnworked penetration after cycle 1 cycle 239 254 245 246 268 247 247of heating at 150.degree. C. for 20 hours 2 cycle 242 254 239 245 268 245 240and cooling by leaving in air 3 cycle 238 260 241 238 274 244 241for 4 hours 4 cycle 233 261 236 237 270 239 235Unworked penetration after cycle 1 cycle 242 263 248 252 265 253 262of heating at 180.degree. C. for 20 hours 2 cycle 260 272 258 254 274 258 272and cooling by leaving in air 3 cycle 273 280 264 261 286 271 279for 4 hours 4 cycle 282 291 277 272 299 283 292Roll stability100.degree. C., 24 hr 297 287 299 280 332 298 298150.degree. C., 24 hr 301 294 303 286 328 304 308__________________________________________________________________________ Example Example Example Example Example Example ExampleTest items 15 16 17 18 19 20 21__________________________________________________________________________Worked penetration 283 280 276 288 283 274 270Dropping point (.degree.C.) 271 261 259 276 269 260 266Oil separation100.degree. C., 24 hr (%) 0.9 1.3 1.3 0.6 0.8 1.2 0.8150.degree. C., 24 hr (%) 1.0 1.1 0.8 0.5 1.2 1.0 0.6Oxidation stability 2.05 2.15 2.15 2.25 2.05 2.20 2.15150.degree. C., 200 hr (kgf/cm.sup.2)Form of grease after test grease- grease- grease- grease- grease- grease- grease- like like like like like like likeWorked penetration of grease after test 289 301 284 300 282 291 293Dropping point of grease after test (.degree.C.) 263 251 250 274 259 270 267Heating-cooling cycle testUnworked penetration after cycle 1 cycle 267 242 251 259 253 234 237of heating at 150.degree. C., for 20 hours 2 cycle 262 248 247 261 255 230 241and cooling by leaving in air 3 cycle 255 242 242 260 254 229 245for 4 hours 4 cycle 248 239 236 253 246 226 256Unworked penetration after cycle 1 cycle 269 249 260 266 255 240 258of heating at 180.degree. C. for 20 hours 2 cycle 272 258 264 274 261 257 263and cooling by leaving in air 3 cycle 278 271 270 283 269 255 271for 4 hours 4 cycle 282 284 274 295 280 274 290Roll stability100.degree. C., 24 hr 313 297 306 318 312 294 309150.degree. C., 24 hr 315 295 315 325 317 298 304__________________________________________________________________________ Example Example Example Example Example Example ExampleTest items 22 23 24 25 26 27 28__________________________________________________________________________Worked penetration 277 281 279 285 280 273 291Dropping point (.degree.C.) 272 275 264 272 268 268 278Oil separation100.degree. C., 24 hr (%) 1.1 0.5 1.6 1.0 1.5 0.8 0.8150.degree. C., 24 hr (%) 1.1 0.9 0.7 0.5 1.2 1.4 0.6Oxidation stability 2.30 2.25 2.05 2.20 2.15 2.30 2.00150.degree. C., 200 hr (kgf/cm.sup.2)Form of grease after test grease- grease- grease- grease- grease- grease- grease- like like like like like like likeWorked penetration of grease after test 293 284 294 293 297 285 295Dropping point of grease after test (.degree.C.) 265 266 253 266 260 254 270Heating-cooling cycle testUnworked penetration after cycle 1 cycle 240 257 252 250 242 240 269of heating at 150.degree. C. for 20 hours 2 cycle 241 253 248 242 238 241 264and cooling by leaving in air 3 cycle 247 246 249 240 235 248 257for 4 hours 4 cycle 250 233 245 233 230 245 250Unworked penetration after cycle 1 cycle 251 267 264 259 252 253 274of heating at 180.degree. C. for 20 hours 2 cycle 261 279 265 268 260 264 284and cooling by leaving in air 3 cycle 273 287 269 278 271 278 291for 4 hours 4 cycle 288 302 268 291 289 299 298Roll stability100.degree. C., 24 hr 313 287 285 316 288 280 302150.degree. C., 24 hr 317 289 285 320 291 279 297__________________________________________________________________________ Example Example Comparative Comparative ComparativeTest items 29 30 Example 1 Example 2 Example__________________________________________________________________________ 3Worked penetration 285 278 283 271 290Dropping point (.degree.C.) 280 269 265 262 271Oil separation100.degree. C., 24 hr (%) 1.2 1.5 1.4 4.6 4.4150.degree. C., 24 hr (%) 1.3 0.7 1.9 3.9 3.6Oxidation stability 1.95 2.05 2.40 4.05 3.15150.degree. C., 200 hr (kgf/cm.sup.2)Form of grease after test grease- grease- liquid liquid liquid like likeWorked penetration of grease after test 292 284 -- -- --Dropping point of grease after test (.degree.C.) 274 258 -- -- --Heating-cooling cycle testUnworked penetration after cycle 1 cycle 248 250 121 125 more than 400of heating at 150.degree. C. for 20 hours 2 cycle 247 245 103 123 more than 400and cooling by leaving in air 3 cycle 242 243 104 120 more than 400for 4 hours 4 cycle 239 240 98 121 more than 400Unworked penetration after cycle 1 cycle 259 260 135 142 more than 400of heating at 180.degree. C. for 20 hours 2 cycle 268 268 127 121 more than 400and cooling by leaving in air 3 cycle 277 271 107 110 more than 400for 4 hours 4 cycle 286 283 92 113 more than 400Roll stability100.degree. C., 24 hr 299 290 230 380 372150.degree. C., 24 hr 294 296 251 more than 400 more than__________________________________________________________________________ 400
When Examples 1-30 are compared with the commercially available prior urea greases of Comparative Examples 1-3, both the oil separation and the roll stability at 100.degree. C. and 150.degree. C. and the oxidation stability at 150.degree. C. in the examples are superior to those of the comparative examples. Concerning the grease form after the test of the oxidation stability, any three comparative examples of the commercially available urea greases are liquid and the grease structure is broken, while all the greases of the present invention maintain the grease form and can expect the lubricating activity at a high temperature for a long period of time.
In the heating-cooling cycle test at 150.degree. C. and 180.degree. C., the consistency of the commercially available urea greases show the noticeable hardening and softening, while the greases of the present invention keep the original consistency and show that the structural stability of the thickening agent of the greases according to the present invention is very high.
Thus, it can be said that the triurea greases according to the present invention are far more excellent in the high temperature properties than the prior urea greases.

Number	Name	Date	Kind
4100081	Dreher et al.	Jul 1978
4113640	Wulfers	Sep 1978

Triurea grease compositions

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