US2211941A - Grease - Google Patents

Description

Patented Aug. 20, 1940 UNITED STATES GREASE Frederick W. Sullivan,

Jr., Augusta, Mich., as-

signor to Standard Oil Company, Chicago, 111., a corporation of Indiana No Drawing. Application November 18, 1938,

' Serial No. 241,261

7 Claims.

This invention relates to an improved method of preparing greases and more particularly to the preparation of greases from nitriles.

I have discovered that greases of improved 5 properties can be prepared from nitriles, particularly long chain alkyl nitriles, otherwise known as alkyl cyanides. The preparation of greases is intimately associated with the refining of petroleum and for this reason it is highly desirable that the constituents used in the preparation of greases be as far as possible, products of petroleum or be prepared from the products of petroleum. Long chain alkyl nitriles for my improved grease can be prepared from paraffin l6 waxes. The parafin wax is first chlorinated by bubbling chlorine gas through the body of the molten wax maintained at a temperature of about 250 F. until the desired degree of chlorination has taken place. I prefer to use the g0 monochlor wax, that is chlorinated Wax having a chlorine content of from about 10% to about 15%, although chlorinated wax containing up to about 50% chlorine can be employed. The chlorinated wax is then reacted with an inorganic 25 cyanide such as, for example, NaCN or Hg(CN)2 to obtain the corresponding alkyl nitrile. When using a neutral cyanide such as Hg(CN)z, C112(CN)2, or K2 Hg(CN)4, a small amount of the isonitrile may be formed together with the alkyl 30 nitrile. The former may be removed by treating with dilute acid without affecting the latter.

35 While it is preferred that the nitrile be prepared from chlorinated wax, nitriles prepared by other methods may be used. For example, nitriles can be prepared from alkyl chlorides in w the manner described by Haas and Marshall in Ind. Eng. Chem. 23, page 352 (1931).

In the preparation of greases from alkyl nitriles according to the present invention the long chain alkyl nitrile (preferably at least 10 carbon atoms) is saponified at a temperature from about 300 F. to about 450 F. in the presence of suflicient alkali or other metal hydroxide and water to complete the reaction and form the soap.

The following examples illustrate the present 50 invention and are not to be considered as limiting the scope thereof.

Example 1.--A soda soap grease was prepared by reacting 86 parts of cetyl nitrile with about 14 parts of sodium hydroxide and a sufiicient 55 amount of water at a reaction temperature of from about 300 F. to about 400 F. until the reaction was completed. The reaction was substantially completed in about 10 minutes but a total time of about 60 minutes was allowed in order to assure complete saponification. The soap obtained was blended with oil at about 200 F. to produce a smooth bright grease similar to cup greases in appearance but having a melting point higher than that of the ordinary soda greases. The melting point of the grease was about 385 F.

Example 2.-A calcium soap grease was prepared by heating a mixture of about 60.6% of cetyl nitrile with about 9.1% calcium hydroxide and about 30.3% Water to a temperature of about 15 340 F. Upon completion of the saponification the calcium soap formed was blended with a mineral lubricating oil at about 200 F. to produce a bright calcium soap grease. I have found it desirable in preparing the calcium soap to carry out the hydrolysis in a pressure vessel in order to avoid excessive loss of water.

Although in the foregoing xamples the greases were prepared by blending the soap with oil after saponification, equally good results are obtained when the oil is blended with the nitrile before saponification. In addition to calcium soap greases. and sodium soap greases other greases, such as a mixture of sodium-calcium greases, aluminum soap greases, lead soap greases, barium soap greases and other metallic soapgreases can be prepared by appropriate modifications of the methods herein described using the metal hy-'- droxides or other metal compounds as saponifying agents.

While I have described my invention by reference to certain preferred embodiments thereof, I do not wish to be limited to the'specific examples which are merely set forth to illustrate my invention and not intended to be a limitation 40 I thereof, except insofar as defined in the appended claims.

I claim: I

1. In the preparation of a grease containing a soap and oil the improvement which comprises preparing the soap by saponifying a long chain alkyl nitrile with a saponifying agent.

2. A method of preparing a grease comprising saponifying a long chain alkyl nitrile with a metal compound saponifying agent to form the corresponding soap and incorporating suflicient mineral lubricating oil to obtain a grease of the desired consistency.

3. A method of preparing a grease comprising saponifying a long chain alkyl nitrile with an 5 alkali and subsequently blending the soap so obtained with a mineral lubricating oil.

4. A method of preparing a grease comprising blending a mineral lubricating oil with a long chain alkyl nitrile and saponifying the said nitrile with an alkali.

5. A method of preparing a grease comprising saponifying cetyl nitrile with caustic soda in the presence of a small amount of water at a temperature from about 300 F. to 400 F., separatlng the soap formed in the saponiflcation from the reaction mass and blending said soap with suificient mineral lubricating oil to obtain a soda soap grease of the desired consistency.

6. A method of preparing a calcium soap grease comprising saponifying cetyl nitrile with calcium hydroxide in the presence of water under pressure at a temperature of about 350 F. whereby a calcium soap is formed and subsequently blending said soap with suflicient mineral lubricating oil to produce a calcium soap grease of the desired consistency.

7. A method of preparing a grease comprising halogenating a paraffin wax, reacting the halogenated paraffin wax with a neutral metallic cyanide to form a long chain alkyl nitrile, reacting said long chain alkyl nitrile with a metal hydroxide in the presence of water to form a soap and incorporating sufiicient mineral lubricating oil to obtain a grease of the desired consistency.

FREDERICK W. SULLIVAN, JR.