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UNITED States PATENT of FICE 239,958 Proouction of Lubricants Harold M

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UNITED States PATENT of FICE 239,958 Proouction of Lubricants Harold M Patented Apr. 9, 1946 2,397.956 UNITED STATEs PATENT of FICE 239,958 PRooUCTION OF LUBRICANTs Harold M. Fraser, New Orleans, La., assignor to Lubieant Corporation, Orleans,International La., a corporation of Louisiana New No Drawing. Application January 15, 1943, Seria No. 42,509 15 Claims. (C. 252-40) The present invention relates to the production by heating a lubricant base, as for example mini of lubricants, and more particularly to lubricants eral oil, vegetable oil, or animal oil or mixture containing a lubricant base, as for example min thereof, or similar oils well known to the art, and eral oil or other equivalent oils well known in the the heating of the mixture is carried to a point art, said lithium soap in the preferred form of above the melting point of the grease, as for ex the invention being a lithium soap of 12-hydroxy ample to 425 F., a firmer and more stable grease stearic acid, or a lithium soap of hydrogenated is produced if the grease is stirred during the time Castor oil. it is cooling from a fluid to a solid or semi-solid It has hitherto been proposed to manufacture state. A grease prepared in the manner above lubricants containing lithium soaps of the fatty 10 set forth which is agitated during the time it is acids, as for example lithium stearate or lithium cooling exhibits less tendency to seep oil. There oleate. However, during the manufacture of fore, in the preferred form of the present inven such greases, difficulties have been experienced in tion, the fluid grease is agitated during the period obtaining sucessive batches of grease having the the grease is cooling.from a liquid to a solid or Same uniform characteristics. For example, in Semi-solid state. More specifically, a firmer the manufacture of a grease containing lithium grease is obtained if the grease is agitated while stearate, one batch of the grease may produce a it is cooled from a fluid state, that is from above relatively hard grease, and the succeeding batch the melting point of the grease to about 275 or may produce a much softer grease. Difficulties in the neighborhood of 200 F. It is desired to of this character are eliminated when the grease 20 point out that it is exceedingly difficult to obtain is made with a lithium soap of a hydroxy stearic a uniform grease of good texture when a lithium acid, and preferably a lithium soap of 12-hydroxy stearate grease is stirred while cooling. When a Stearic acid, or a lithium soap of hydrogenated lithium stearate grease solidifles, it assumes a Castor oil. In general, it may be stated when very stiff state, and if any attempt is made to stir greases are manufactured with lithium Soaps of it, the grease becomes ropy and separates into the character above pointed out, the resulting lumps of grease of very poor quality. greases have more uniform characteristics. In the preferred form of the invention, the It also has been discovered that a grease con greases containing the lithium soap of hydroxy taining a lithium soap of hydroxy stearic acid, stearic acid, and preferably the lithium soap of and particularly the lithium soap of 12-hydroxy 30 12-hydroxy stearic acid, are during the process stearic acid, or the lithium soap of hydrogenated of manufacture heated to a point to substantially castor oil, possesses exceedingly high mechanical dehydrate the grease, that is, so the grease will stability. After mechanical working, greases contain less than 0.025% to 0.5%, and preferably containing lithium soaps of the above character less than 0.025% of water. If the greases pre have a substantially greater consistency than 35 pared as herein Set forth are heated above 400 greases worked to a similar extent which contain F., and usually between 400 to 425 F., practically lithium stearate, oleate, or other lithium fatty all of the water present is driven off and the , acids. In other words, greases containing the grease then is substantially dehydrated. If the lithium soap of hydroxy stearic acid, and es grease is heated to temperatures below 400 F., pecially the lithium soap of 12-hydroxy stearic 40 varying amounts of water are left in the grease. \cd. or the lithium soap of hydrogenated castor It has also been ascertained that greases con oil, retain their consistency over a long periods taining the lithium soaps of hydroxy stearic f mechanical working, whereas similar greases acid, and particularly 12-hydroxy stearic acid, containing the lithium soap of stearic acid or and greases containing the lithium soap of hy oleic acid and similar fatty acids deteriorate in 45 drogenated castor oil as originally produced, have mechanical consistency. One field in which the a rather grainy or coffee grounds appearance, greases of the present invention have given excel but that this grease can be converted to a smooth lent results is in the lubrication of ball bearings buttery texture by milling the grease by any suit where a lubrication is needed which will not drip able milling method, but preferably in accordance from the bearing due to change in consistency 50 with the method set forth in my U. S. Patent from mechanical working. 2,257,945. It has also been discovered that if a lithium It has also been discovered that greases con soap of hydroxy stearic acid, and especially 12 taining a lithium soap made by reacting a lith hydroxy stearic acid, and a lithium soap of hy ium compound with a fatty acid of hydrogenated drogenated castor oil is formed in situ in a grease castor oil exhibit a much better inhibition against 2 2,397,956 oxidation with phenylenediamine and especially as it produces a firmer, more uniform grease hav metaphenylenediamine than when the grease is ing a less tendency to seep oil than if agitation made with a lithium soap produced by reacting had been omitted. The grease is allowed to cool a lithium compound with hydrogenated castor to about 275 and then dumped into a metal pan oil or hydrogenated glyceryl ricinoleate or ricin where it is allowed to cool to room temperature. oleates, or glyceryl 12-hydroxy stearate or stea If the grease is stirred in the kettle to a suffi rates. When the lithium compound is reacted ciently low temperature, it can be filled directly with the latter compounds, a small amount of: into shipping containers. However, it is pre glycerine is produced and the difference in the ferred to dump the grease into the cooling pans action of the anti-oxidant is probably due to the O and thereafter when the grease is cold mill and presence of the glycerine. filter the grease in accordance with the method The present invention in one form is directed set forth in U. S. Patent 2,257,945. The pans are to the production of a grease containing a plu usually filled to a depth of about three inches. rality of soaps, one of the soaps being a lithium When the batch, compounded as above set forth, soap of hydroxy stearic acid, and especially a 5 is poured into a pan in three inch layers, the lithium soap of 12-hydroxy stearic acid or a lith grease cools to room temperature in about six ium soap of hydrogenated castor oil. More par to ten hours. It is highly desirable to control ticularly, the grease may contain in addition to the cooling rate of the grease down to 275 F. the lithium soap herein set forth a sodium soap However, after the grease has been stirred or of a higher fatty acid such as sodium stearate agitated at a temperature from above 275 to or oleate, or a calcium soap of a higher fatty about 275 F, the cooling rate does not become acid, or lithium soap of a higher fatty acid. of great importance. However, if the stirring In producing greases in accordance with the of the grease is continued from about 250 F. present invention, any substantially completely to about 225 F., a much firmer grease is pro hydrogenated castor oil or hydrogenated castor duced.The following table shows. the . effect of agita oil fatty acids may be used, the latter being pro tion while cooling on the worked penetration of duced by splitting hydrogenated castor oil. Ex the grease: cellent results have been obtained by using hy TABLE drogenated castor oil and hydrogenated castor oil fatty acids having the properties set forth in the following table: Temperature.-----------Batch No.--------------- 420() F-300F(2) 250°F,(3) 200(4) F-150(5) F. AB A. S. T. M. work hydrogenated: 35 penetration.----------- 210 187 181 181 185 castor oil fits The results set forth in Table II were obtained Percent free fatty acids................ 1.4 88 in the following manner. A large sample of the Saponification value-- - 18 188 grease compounded as herein set forth was melt Iodine value---------- 2.7 4, 6 40 ed at 425' F. A portion of this large sample was Titre------------------ 74.2 69 poured at 420 while liquid. This grease, iden In producing the lithium soap from the hy tified as batch No. 1 in Table II, had not been drogenated castor oil or the fatty acid of hydro stirred and had a worked penetration of 210. genated castor oil above set forth, any suitable Another batch of the grease which had been lithium compound may be used, including lithium 45. compounded at 425 F. was stirred down to 300 hydroxide, lithium carbonate, lithium oxide and F.
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