US2870089A - Open gear lubricants - Google Patents

Description

Jan. 20, 1959 J. F. MGGROGAN 2,870,089

OPEN GEAR LUBRICANTS Filed Oct. 29, 1956 INVENTOR. JOHN F. Mc GROGAN %Z.Z Z

ATTORNEY OPEN GEAR LUBRICANTS Application October 29, 1956, Serial No. 618,949 Claims. (Cl; 252-42) This invention relates to novel lubricants and method for their manufacture. More particularly, itis concerned with opengear lubricants which are widely used on the large, slow-moving open gears, cable drums, drag chains and other similar equipment usually foundin the steel, coal, cement and construction industries.

Open gear lubricants are a distinct class of lubricants which are generally composed of residual petroleum stocks. The lubricants of the instant invention are unique in that the residual asphalts are thickened by a minimum amount of sodium soap which is formed in the lubricant in a novel way during processing. These new lubricants are superior in important characteristics such as. high dropping point, retention of lubricant at elevated temperatures, coverage, tackiness, and lubricity at high loads. They are suited to. the various methods of. application currently used and provide adequate lubricating for extreme pressure use under heavily loaded. conditions, as well. as for normal service.

Itv is therefore an object of this invention to provide a novel method of manufacturing open gear lubricating greases;

It is another object of this invention to provide. open gear lubricants. possessing high dropping point characteristics while still maintainingrelatively soft penetration characteristics.

It is another object of this invention. to provide open gear lubricants possessing high temperature. retention characteristics, having high retention in static areas and flowing more freely in the gear teeth.

It is still another object of this invention to provide open gear lubricants which remain plastic and tacky at very low temperatures, and which may be applied by paddle or brush or which may be readily sprayed or poured at existing ambient temperatures.

It is a further object ofthis invention to provide open gear lubricants having extreme pressure propertieswhich provide adequate lubrication under heavily loaded conditi-ons.

Other objects and advantages will become apparent from a reading of the specification and the appended claims.

In accordance with the present invention, it has been discovered that open gear lubricants having'these desired properties may be produced by forming in situ a small amount of sodium soap in a major amount of a residual steam refined asphalt at a temperature of from approximately 190 F. to approximately 205 F., affecting a. high degree of dispersion of the soap in the asphalt during and after saponification and further processing the soapthickened asphalt at a temperature of from approximately 210 F. to 240 F. The desired degree of dispersion is accomplished by mechanically mixing the components with a mixer giving a high degree of dispersion such as the so-called lightning" mixer, While at the same time continuously bubbling air through the reaction massby means of an air spider or similar distributing mechanism and by continuously removing aportion of rates atent ice 2. the mixture from. the main reaction mass, pumping it through a strainer (preferably of .about mesh size). by meansv of a. gear pump'and recycling theremoved portion ofv themixtureto-the main-reaction mass- Mixing, air blowing and. recyclingv is continued while processingatZlO. F-..t o.2.40. F. until thematerial. reaches the desiredASTM dropping point and penetration ranges, whichmaterial will. hereinafter be termed the basegrade lubricant. The desired ASTM dropping'points are 300*" and higher,.while. the desired ASTM- penetration unworked. at 77 'F. ranges preferably from to- 230.

Fora betterunderstanding of the processutowhich this'invention'is directed, reference shouldbe had to the accompanying drawing which illustrates the process set forth above- A reaction vessel 1 is provided with a. stirring means 2 andairline Sto-anair; distributing means 4 located at the bottom ofthe reaction vessel 1. Reactant inlet lines 5, 6'; and 7 for admittingasphalt, fatty acid, and. sodium hydroxideresp'ectively are provided for the purpose of introducing'the. reactants: into the. vessel. A withdrawalline 8 at 'the'bottomof the reaction vessel 1. is provided with avalve 9 for eithercompletel'y withdrawing the reactant mixture. through line 10 or con-' tinuously. recycling a portion of the reactant mixture through line. 11,, gear pump 12, strainer 13' and recycle line 14;. backinto vessel 1.

To produce solventstliinned grade lubricants from two weight percent to 40- weight percent (based on the total mixture) of. Stoddarck solvent or similar petroleum solvent is. added to the base grade" lubricant, but it is preferable to add about 1.0 weight percent solvent for summer: use and about 13 weight percent for winter use. The'penetration of the solvent-thinned grades rangesfrom 320 to 400 for'tlie grades which contain from 10 per cent to. 1-3 percent thinning solvent. Base grades are generally applied with paddle or brush after being moderately heated tov about 150 F. to 200 F. The solvent-thinned gradeszmay be applied by spraying, brushing, or pouring at existing ambient temperatures.

Prior to the instant invention resort was usually had to a pre-oxidized asphalt which was then thickened with a. relatively large. amount. of soap in order to obtain greases having relatively high dropping points. This necessitated airblowing' the asphalt for a prolonged period; of time. at excessively high temperatures ranging from 450 F. to 600 R, which treatment not only required special and expensive'equipment butalso tended to degrade the asphalt by oxidation.

It was found that. only a minimum amount of soap is required to thicken the asphalt to the desired dropping point by forming thesodium soap in situ in the residual asphalt and dispersing said soap by the novel manner of this invention. From one weight percent tofive weight percent of the, sodium soap formed in. from 95 weight percent to 99 weight percent of the asphalt. is. suitable for this purpose, although from two weight per cent to three weight percent of the soap is preferred. Moreover, by simultaneously mixing, air blowing, and recycling the components a high degree of dispersion of the formed soap in the asphalt is effected so that the desired high dropping point isattained in a relatively short period of time and the tively lowtemperatures ranging between approximately 190 F. to 240 F. andrequiring no special equipment other than the ordinary equipment normally used to produce greases.

The airblowing dispersion of the soap, hastens the removal of water and it partially oxidizes the asphalt so as to produce a product which has the: desiredhbody characteristics. at elevated temperatures. It is to be noted, however, that the asphalt" process may be carried on at rela-' has a threefoldeffect. It promotes the is not oxidized to the point of quality degradation. The in sun formation of the sodium soap in the asphalt and arr blowing the mixture at a relatively low temperature result in a more efiicient process than those used in the past in that all of the formed soap immediately has'an effect on the thickening of the asphalt,'whereas by prevlous methods of pre-oxidizing the asphalt and adding soap, a portion of the soap initially added would not have any effect on the thickening of the asphalt. Hence, by the process of this invention a minimum amount of soap is required to reach the desired dropping point.

The No. 2 saturant grade asphalt used in the instant invention is preferably a residual asphalt from a steam refined Venezuelan, Bachaquero or Lagunillas crude. These crudes are low gravity, low pour point, high sulfur content, high residual content, asphaltic type crndes. The Islo. 2 saturant grade has the following ASTM specificatrons:

D70 specific gravity e 0990+. D-92 flash, F 350 Min. D-6 loss (50 grams, hrs. at 325 F.) percent 5 Max. D-139 float at 122 F 100-150 secs.

These No. 2 saturant grade asphalts were analyzed by the method .of Rostler and Sternberg in order to characterize them further. This method of analysis is described in the following publications: Industrial and Engineering Chemistry, 1949, volume 41, No. 5, page 598; Rubber Age, 1951, volume 67, No. 5, page 559; Rubber Age, 1952, volume 70, page 735. It essentially comprises successively contacting the selected oil with (1) hexane, (2) 85% H 80 (3) 95% H S0 and (4) 120% H 80 That portion of the oil which is insoluble in hexane (or precipitates therefrom) is deemed to be asphaltenes; that portion of the remaining oil which reacts with 85% H 80 is deemed to be N-base resins; that portion of the remaining oil which reacts with 95 percent H 50 is deemed to be group I resins; that portion of the remaining oil which reacts with 120 percent H 80 is deemed to be groupII resins; and that portion of the original oil which is not reacted upon by any of the foregoing treatments is deemed to be composed of parafiinic hydrocarbons.

A number of asphalts had the following composition ranges by the Rostler and Sternberg method of analysis:

Weight Weight Weight Weight Weight Percent Percent Percent Percent Percent Asphait- N-Base GronpI GroupII Saturated enes Resins Resins Resins Hydrocarbons Lazunillas saturant No.2 11.0-12.2 21.121.8 16.7-17.2 30. 8-318 18.1-19.9 Bachaquero saturant;

A typical Lagunillas No. the following characteristics:

Rostler and Sternberg analysis in percent by weight The fatty acids used to form the sodium soap in the instant invention include both animal and vegetable saturated fatty acids, such as palmitic acid, stearic acid,

2 saturant grade asphalt had I etc. In general, the saturated fatty acids having from 14 to 24 carbon atoms in the molecule are satisfactory with those having from 16 to 22 carbons being preferred. Fats, as well as fatty acids, also may be used to form the soap, but fatty acids are preferred because of their more rapid reaction (saponification) rate. From about 0.88 weight percent to about 4.39 weight percent of the fatty acid may be used, but it is preferred to utilize about 2.0 to 3.0 weight percent of the fatty acid. The preferred fatty acid among those used is known commercially as Hydrogenated Hydrex, and is composed of hydrogenated marine fatty acids. It has the following specifications:

Iodine value 10 Maximum.

Saponification number 195 Minimum. Free fatty acids,

as percent oleic 96 Minimum. Titre, C 53 Minimum. Appearance No dirt, no free water. Odor, typical Mild.

Commercial grade sodium hydroxide may be used for the saponification step. It is preferred to utilize an aqueous caustic solution. Various concentrations of alkali solutions may be employed. A 25 weight percent NaOH solution was found to be satisfactory. From about 0.12 weight percent to about 0.61 weight percent of sodium hydroxide (on a dry basis) may be used, but it is preferred to utilize about 0.3 weight percent to 0.4 weight percent of sodium hydroxide.

The solvent used for preparing the solvent thinned grade lubricants of the instant invention should have a moderate initial boiling point and be falrly'close-cut in order to give an even evaporation rate in use. Any petroleum distillate having these characteristics may be used. A commercial petroleum distillate known as Stoddard solvent was found to have the desired characteristics. It had the following analysis, which analysis, however, should only be considered as a typical analysis of a suitable solvent since other solvents with somewhat higher and lower boiling ranges are equally efiective.

ASTM D-287 API gravity at F 48.5

ASTM D-56 flash point T. C. 0., F 104 ASTM D-86 distillation:

Initial boiling point F 305 10% boiling point F 315 30% boiling point F 320 50% boiling point F 325 boiling point F 330 boiling point F 345 End point 375 It has been discovered that extreme pressure properties can be imparted to the base grade lubricants of this invention by incorporating therein certain proportions of graphite and a methyl ester of lard oil. It is known in the prior art that certain substances, especially those which contain as the active ingredient either sulfur, chlorine, lead, or phosphorous compounds or mixtures of. these compounds, greatly augment the load carrying capacity of lubricating compositions. It is theorized that under high pressure between metal surfaces these chemical elements react with the metal to produce a coating which will sustain the load or prevent the two metals from welding together, thus precluding damage to the mechanical parts.

To test the extreme pressure properties of an industrial lubricant of the type disclosed in the instant invention the Four-Gram Tirnken Test was developed by the United States Steel Company as a standard test. This test is described in the United States Steel Companys Lubrication Engineers Manual. Essentially the test is conducted in a machine in which a test cup is rotated againsta steel test block. A four gram sample of the grease undertest is applied by spatula to the bearing sur It is preferred face of the test cup and block. The machine is rotated by hand until the excess grease on the" cup has been removed by the test block. Pressures between the test members are regulated by applying a suitable load to lever arms. The test is run under a 43 pound lever load at a mandrel speed of 800 R. P. M. for a period of 30 minutes. Failure is indicated by the appearance of the lubricant film on. the test cup or by machine chatter, smoke, overheating, or sounds that indicate d'ry metal pick up. A lubricant which supports the 43 pound lever load for at least 30 minutes without failure is considered to be satisfactory for use under'heavily loaded conditions.

The extreme pressure additives normally used inthe prior art were not effective when incorporated in the base grade lubricants of the instant invention. Lead naphthenate tended to de-gel the lubricant which resulted in a. lowering of the dropping point. The base grade lubricants of this invention containing chlorinated compounds and also those containing sulfurized oils failed to pass the Timken test. The addition to the base grade lubricants of Methyl Lard'ate', a commercial methyl ester of lard oil fatty acids, gave good results in the Timken test although the Timken cup appeared to be bare during; the test. In order to gain better coverage, graphite was added to the Methyl Lardate containing composition. It was discovered that the combination of these two ingredients not only improved the coverage but extended the running time of the Timken test to beyond 45 minutes, the latter discovery being quite unexpected since neither of these materials normally are considered to be extreme pressure additives. From one weight percent to four weight percent graphite may be added, the preferred range being from two weight percent to three weight percent based 'on the. total composition. The amount of Methyl Lardate may vary from 0.5- weight percent to weight percent based'on the-total composition, one to two weight percent being the preferred range.

The graphite employed in the instant invention as an extreme pressure additive may be obtained commercially. to utilize a small particle size graphite. A naturally occurring" small particle size graphite known commercially as lettinos'No. 5'4'69 graphite was found to besuitable inimproving theTimken' test results. In addition it provides a darker coating on the lubricated surface.

The other extremepressure additive used in the. instant invention in conjunction with the graphite is a methyl ester of lard oil known commercially as Methyl Lardate. It has the following typical characteristicsz.

Titre 30 C. Flash, C. O. C 345 F. Fire, C. O. C 380 F. Pour point 45 F. Saponification value 195 Iodine value 75 It has also been found that the base grade lubricants may be combined'with certain petroleum lubricating oil distillates to produce lubricantsro-f high dropping points but increased penetration characteristics. Likewise, the

base grade lubricantto which has been added the. aforementioned extreme pressure additives may be combined With the lubricating oil distillates to increase thepenetration characteristics of the grease.

The preferred lubricating oil distillates are those having Saybolt Universal viscosities of between 90 and 110 seconds at 100 F. and A. P. I. gravities at 60 F. of about 25 F. It is also preferable that the distillates be naphthenic in character since such oils are more compatible with the asphaltic base. One such oil which isknown in the petroleum industry as 100 Coastal Oil has been found to be highly satisfactory for this purpose in amounts ranging up to 1'5 to 20 percent by weight of the final composition.

. If desired, either thebase grade lubricant towhichhas been added the above described lubricating. oil distillate or the base grade lubricant containing the extreme pressure additives to which has been added the lubricating oildisti'llate may also be thinned by the addition of the above described petroleum solvents such as Stoddard solvent in amounts between 2 and 40 weight percent.

The open gear lubricants of the instant invention are tested for dropping point characteristics using the ASTM test procedure designated as D-566. The penetration unworked is tested according to ASTM D-217 with the following modifications:

For the base grade lubricants, the moderately heated sample (150 F.) is'transferred to a 6 ounce penetration tin and is placed into a 77 F. bath overnight before the penetration is taken.

For the solvent-thinned lubricants, the sample is' transferred to a one-pound grease can of 3% inches diameter and allowed to stay in 77 F. bath overnight before the penetration is taken. p

The four-gram Tirnken test, previously described, when applied to the extreme pressure gradelubricants is run for a. minimum period of. 30 minutes under a lever arm load of 43 pounds at a mandrel. speed of 800 R. P. M.

The ASTM dropping point is the most significant of the characteristics and is used as a control test during processing since it is. really an indication of the degree of dispersion of the soap in the asphalt. The lubricants of the instant invention have a dropping point of from 300 F. to 400 F., preferably, although slightly lower or higher dropping points are not objectionable.

Theunworked penetrations of the base grade lubricants range from 190 to Eli-minimum. The 10 percent solventthinned grades have unwo-rked penetrations of 320 to 350 minimum, while the 13 percent solvcnt-thinned grades range f'ronr360 to 400 minimum.

The in situ formation of the sodium soap in the asphalt and the method for its homogeneous dispersion which form a part ofthe instant invention result in products possessing unique characteristics. One such. characteristic is its unique behavior under low shear rates. This is demonstrated by comparing pressure viscosities obtained on the unmodified No. 2 saturant grade asphalt against the soap thickened material, whichv is-- the base grade open gear lubricant of this invention.

TABLE I Apparent Viscosity in Poises Shear Rate Tempp, F. (Reciprocal i Seconds) No. 2 Open Gear Saturant Lubricant Base The pressure viscosity data were obtained according to ASTM method 13-1092 except that the apparatus was enclosed in a thermostattcd cabinet and the viscosities were obtained at two elevated empcratures, 120 F. and l50'F.'.. Atlow shear rates the open gear lubricant-is much more viscous than the saturant from which it is made; while at higher shear rates, thevi'scosities approach each other. This means that when in service the soap thickened material would have high retention in static areas, while in the gear teeth under high shear conditions the -rnaterial would flow more readily to provide the film of lubricant that isneeded."

. Theliigh' temperature retention properties of the open gear lubricants of this invention are evidenced further by the vertical plate'retention test (adhesion test). In this test the thickness of the lubricant coating on a steel plate either the No. 2 are made, or the commercial solvent-thinned residual is recorded after exposure to elevated temperatures. The

following table gives comparative data obtained on the open gear lubricant, the No. 2 saturant grade asphalt, and a commercial solvent-thinned residual asphalt type grease.

This data shows the products of the instant invention have better high temperature retention characteristics than saturant grade asphalt from which they asphalt type greases.

The products of the instant invention remain plastic at very low temperatures as evidenced by a low temperature flexing test. In this test, a strip of heavy aluminum foil is coated with the lubricant and placed into a cold box where the temperature is lowered in ten degree steps. At each step the lubricant coated aluminum strip is flexed. The temperature at which the lubricant cracks and flakes off is its minimum useful temperature. This value was determined to be 10 F. for the base grade lubricants of this invention and 40 F. for the solvent-thinned grades.

The instant invention may be further illustrated by the following examples:

Example I A 5718 pound charge of No. 2 saturant grade asphalt was pumped into a grease kettle and heated by steam to a temperature of 150 F. to 190 F. The lightning mixer and the recycle gear pump were started and the air blower turned on. A 150 pound charge of hydrogenated marine fatty acids (Hydrogenated Hydrex) was added to the kettle and the steam was adjusted to raise the kettle temperature to 190 F. to 195 F. A 25 percent solution of NaOH containing 21 pounds NaOH on a dry basis was added to the kettle. Saponification was carried on for a period of two hours at a temperature of 190 F. to 195 F. The temperature was increased to 225 F. to 230 F., while the mixing, recycling and air blowing were continued. Air blowing was intermittently stopped for the incremental addition of 152 pounds of Pettinos No. 5469 graphite. After the addition of 61 pounds of,Methyl Lardate, mixing, recycling, and air blowing were continued at a temperature of 230 F. until the lubricant had an ASTM dropping point of 360 F. Heating and air blowing were discontinued at this stage. The lubricant had the following composition, in Weight percent, at this point in its manufacture:

No. 2 saturant grade asphalt; 93.7 Hydrogenated marine fatty acids (Hydrogenated Hydrex) 2.46 Sodium hydroxide (dry basis) 0.34 Graphite, No. 5469 2.5 Methyl Lat-date (methyl ester of lard oil) 1.0

A four-gram Timken extreme pressure test was run on the lubricant for thirty minutes without evidence of failure.

Example II Weight percent No. 2 saturant grade asphalt 97.5 Hydrogenated marine fatty acids (Hydrogenated Hydrex) Sodium hydroxide (dry basis) The above composition produced as in Example II had an ASTM dropping point of 313 F. and an unworked penetration at 77 F. of 210.

Example IV Weight percent No. 2 saturant grade asphalt 87.48 Hydrogenated marine fatty acids (Hydrogenated Hydrex) 2.21 .Sodium hydroxide (dry basis) 0.31 Stoddard solvent 10.0

The above composition produced by the method of Example II, except for the addition of solvent, had an ASTM dropping point of 331 F. and a penetration, unworked, at 77 F. of 358.

Example V Weight percent No. 2 saturant grade asphalt 81.52 Hydrogenated marine fatty acids (Hydrogenated Hydrex) 2.14 Sodium hydroxide (dry basis) 0.30 Graphite, No. 5469 2.17 Methyl Lardate (methyl ester of lard oil) 0.87 Stoddard solvent 13.00

Example VI A portion of grease made in accordance with the pro cedure of Example I and containing exactly the same percentage of ingredients with the exception that no Stoddard solvent was added, was combined with 15 percent by weight, based on the final composition, of a Coastal oil containing 2.5 percent by weight of graphite and 1.0 percent by weight of Methyl Lardate.

The final composition, in percent by weight, was as This grease had an unworked penetration of 319 (aver.- age) at 77 F. and passed the Four-Gram Timken extreme pressure test (over 30 minutes without failure).

"In general, the amountsof'the arious ingredientsof the'compositions of the instant invention lie within the following ranges in percent by weight:

While this invention has been described with reference to specific examples and details of the production and properties of the compositions of the instant invention, it is to be understood that it is not intended to limit the invention to such specific examples and details, except as hereinafter recited in the appended claims.

I claim:

1. A lubricating grease consisting essentially of a major amount of a partially oxidized liquid residual asphalt and a minor amount, sufiicient to thicken said asphalt, of the reaction products formed in said asphalt of an hydrogenated marine fatty acid and sodium hydroxide.

2. A lubricating grease consisting essentially of a partially oxidized mixture of the following ingredients in percent by weight based on the grease:

No. 2 saturant grade asphalt 95-99 Hydrogenated marine fatty acids 0.88-4.39 Sodium hydroxide (dry basis) 0.12-0.61

3. A lubricating grease consisting essentially of a major amount of the composition of claim 2 and from about 2 Weight percent to about 40 weight percent based on the final composition of a petroleum solvent.

4. A lubricating grease consisting essentially of from about 87 weight percent to about 90 weight percent of the composition of claim 2 and from about 10 to about 13 weight percent of a petroleum solvent.

5. A lubricating grease consisting essentially of a major amount of the grease of claim 2 and up to 20 Weight percent based on the final composition of a petroleum lubricating oil distillate.

6. A lubricating grease consisting essentially of from about 60 to about 98 weight percent of the composition of claim 5 and from about 40 to about 2 weight percent of a petroleum solvent.

7. A lubrication grease having extreme pressure properties consisting essentially of a major amount of a partially oxidized liquid residual asphalt and a minor amount, sufficient to thicken said asphalt, of the reaction products formed in said asphalt of hydrogenated marine fatty acids and sodium hydroxide, together with graphite and a methyl ester of lard oil, in minor but in sufficient amounts to impart extreme pressure properties to the thickened asphalt.

8. A lubricating grease having extreme pressure properties consisting essentially of a partially oxidized mixture of the following ingredients in percent by weight based on the grease:

No. 2 saturant grade asphalt 95-99 Hydrogenated marine fatty acids 0.88-4.39 Sodium hydroxide (dry basis) 0.12-0.61 Graphite 1-4 Methyl ester of lard oil 0.5-5

9. A lubricating grease consisting essentially of a major amount of the composition of claim 8 and from about 2 weight percent to about 40 weight percent based on the total composition of a petroleum solvent.

10. A lubricating grease having extreme pressure prop erties consisting essentially of a major amount of the grease of claim 8 and up to 20 weight percent, based on the final composition, of a petroleum lubricating oil distillate.

11. A lubricating grease having extreme pressure properties consisting essentially of from about to about 98 weight percent of the composition. of claimv 10 and from about 40 to about 2weight percent of apetroleum solvent.

12. A process for the manufacture of a lubricating grease which comprises saponifying in a major amount of a liquid residual asphalt minor amounts, sufficient to thicken said asphalt, of an hydrogenated marine fatty acid with sodium hydroxide at a temperature of from approximately 190 F. to approximately 205 F, air blowing, mixing andrecycling the reaction mixture during saponification until a high degree of dispersion of the soap in said asphalt is accomplished, and continuing said air blowing, mixing and recycling at a tempe-rature of from approximately 210 F. to approximately 240 F. until an ASTM dropping point of at least 300 F. and an unworked penetration at 77 F. ranging from about 190 F. to about 230 F. are attained.

13. A process for the manufacture of a lubricating grease which comprises saponifying in a major amount of a liquid residual asphalt minor amounts, sufiicient to thicken said asphalt, of an hydrogenated marine fatty acid with sodium hydroxide at a temperature of from approximately 190 F. to approximately 205 F., air blowing, mixing and recycling the reaction mixture during saponification until a high degree of dispersion of the soap in said asphalt is accomplished, continuing said air blowing, mixing and recycling at a temperature of from approximately 210 F. to approximately 240 F. until an ASTM dropping point of at least 300 F. and an unworked penetration at 7 70 F. ranging from about 190 F. to about 230 F. are attained, discontinuing heating and air blowing and adding from about 2 weight percent to about 40 weight percent of a petroleum solvent.

14. A process for the manufacture of a lubricating grease which comprises saponifying in from about 95 weight percent to about 99 weight percent of a liquid residual asphalt about 0.88 weight percent to about 4.39 weight percent of an hydrogenated marine fatty acid with from about 0.12 weight percent to about 0.61 weight percent of sodium hydroxide at a temperature of from approximately 190 F. to approximately 205 F., air blowing, mixing and recycling the reaction mixture during saponification until a high degree of dispersion of the soap in said asphalt is accomplished, continuing said air blowing, mixing and recycling at a temperature of from approximately 210 F. to approximately 240 F. until an ASTM dropping point of at least 300 F. and an unworked penetration at 77 F. ranging from about 190 F. to about 230 F. are attained.

15. A process for themanufacture of a lubricating grease having extreme pressure properties which comprises saponifying in from about 95 weight percent to about 99 weight percent of a liquid residual asphalt about 0.88 weight percent to about 4.39 weight percent of an hydrogenated marine fatty acid with from about 0.12 weight percent to about 0.61 weight percent of sodium hydroxide at a temperature of from approximately F. to approximately 205 F., air blowing, mixing and recycling the reaction mixture during saponification until a high degree of dispersion of the soap in said asphalt is accomplished, continuing said air blowing, mixing and recycling at a temperature of from approximately 210 F. to approximately 240 F., adding incrementally from about 1 weight percent to about 4 weight percent of graphite with air blowing stopped during said additions, adding from about 0.5 weight percent to about 5 weight percent of a methyl ester of lard oil, and continuing heating, air blowing, mixing and recycling until an ASTM dropping point of at least 300 F. and an unworked penetration at 77 F. ranging from about 190 F. to about 230 F. are attained.

(References on following page) UNITED STATES PATENTS Manley Aug. 25, 1925 Brunstrum er a1. Aug. 20, 1940 Roehner et a1 Nov. 26, 1940 Gothard et al June 17, 1941 Morway et al. 2,625,510 Moore Ian. 22, 1952 Jan. 13, 1953 OTHER REFERENCES plication of Lubricating b. Corp. (N. Y.), 1954,

UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No 2 ,8'70 ,089 January 20, 1959 John F. McGrogan It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction and that the said Letters Patent should read as corrected below.

Column 5, line 66, for "25 F." read 25 column 9, line 47, for

"lubrication" read u lubricating column 10, line 32, for "770 F." read m 77 F. --n

Signed and sealed this 12th day of May 1959.

(SEAL) Attest:

KARL Ho AXLINE ROBERT C. WATSON Attesting Oflicer I Commissioner of Patents

Claims (1)

1. 7. A LUBRICATION GREASE HAVING EXTREME PRESSURE PROPERTIES CONSISTING ESSENTIALLY OF A MAJOR AMOUNT OF A PARTIALLY OXIDIZED LIQUID RESIDUAL ASPHALT AND A MINOR AMOUNT, SUFFICIENT TO THICKEN SAID ASPHALT, OF THE REACTION PRODUCTS FORMED IN SAID ASPHALT OF HYDROGENATED MARINE FATTY ACIDS AND SODIUM HYDROXIDE, TO GETHER WITH GRAPHITE AND A METHYL ESTER OF LARD OIL, IN MINOR BUT IN SUFFICIENT AMOUNTS TO IMPART EXTREME PRESSURE PROPERTIES TO THE THICKENED ASPHALT.

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