US1194013A - Method of refining wool-grease - Google Patents

Description

UNITED STATES PATENT OFFICE.

JAMES O. HANDY AND ROBERT M. ISHAM, OF PITTSBURGH, PENNSYLVANIA, ASSIGN- ORS TO PITTSBURGH TESTING LABORATORY, OF PITTSBURGH, PENNSYLVANIA, A

CORPORATION OF PENNSYLVANIA.

METHOD OF REFINING WOOL-GREASE.

No Drawing.

To all whom it may concern:

Be it known that we, JAMES O. HANDY and ROBERT M. ISHAM, both citizens of the United States, residing at Pittsburgh, Allegheny county, Pennsylvania, have invented a new and useful Method of Refining Wool- Grease, of which the following is a full, clear, and exact description.

Our invention has relation to an improved method of refining Wool grease to obtain what is known as neutral wool grease or lanolin. These products are used largely in the leather industry, the lubricating oil industry, and in pharmacy.

The wool grease available for our method of treatment is of two kinds, namely: naphtha extracted grease obtained by treatment of the raw wool with naphtha, and brown wool grease, or degras, obtained by acidification of the soapy water obtained in the usual processes of wool scouring. The naphtha extracted grease is of a lighter color and contains less free fatty acids, while the other product contains all the fatty acids which were in the soap. Our method of refining is applicable to both these products,

although we preferably use the naphtha ex tracted grease.

The refining problem consists in the removal of the free fatty acids, together with a small portion of the neutral grease, to produce a product which bleaches readily to a yellow color, is neutral, and which consists chiefly of the waxy portion of the original grease. This problem is a diflicult one, because of the tendency of the grease when stirred with Watery liquids to form a resistant emulsion therewith.

It has been usual in the prior art to first neutralize or saponify the grease by the use of an alkali (soda of potash) in an amount slightly in excess of the quantity required to combine with the free fatty acids. The next step has been the separation of the soap thus produced from the neutral Wool grease which it is desired to recover. If the mixture is placed in water, or if water is added to the mixture and the mass is stirred, an

emulsion will be formed even before all the Specification of Letters Patent.

Patented Aug. 8, 1916.

Application filed April 22, 1916. Serial No. 92,843.

soap is dissolved. The solution of the soap is also hindered by the stiff consistency of the wool grease itself.

By our present invention, instead of attempting to remove the free fatty acids by saponification with a fixed alkali and recoyering as a by-product either soap or fatty acids from soap, we completely neutralize the free fatty acids by the use of a volatile base, viz., ammonia.

In carrying out our invention we dissolve the Wool grease in petrolic ether, preferably in the proportion of one kilogram of grease per gallon of petrolic ether, or approximately one-half gallon of solvent per pound of grease. This solution is preferably made 1n a cone bottom tank having a stirring device. To this grease solution is added about one quart 1 wood alcohol or its equivalent, such as denatured grain alcohol, containing in solution from 10 to 12 per cent. of strong ammonium hydrate. The amount of ammonia in the alcohol may, however, be varied beyond the limits mentioned. The two liquids are thoroughly blended together by stirring, preferably for about ten minutes, and are then allowed to separate. The alcoholic liquid containing most of the free fatty acids settles to the bottom of the tank and is drawn off. The petrolic ether solution remaining in the vessel is treated with a second portion of ammoniacal alcohol, preferably of about one-half the strength of the first portion. The ammoniacal alcohol is preferably applied cold, thereby insuring a stable ammonia compound.

The petrolic ether solution remaining after the second alcohol treatment contains only neutral wool grease. It is ready for bleaching with fullers earth. This may be very readily done by agitating it with fullers earth in an amount approximately equal to the weight of the grease. Greatly superior results are obtained by treating the grease with fullers earth while it is in a petrolic ether solution, as fully described in the copending application of James 0. Handy, one of the applicants herein, Serial No. 92,845, filed April 22, 1916.

Any contained ammonia in the petrolic ether solution of neutral wool grease. and which. though small in amount, gives a disagreeable odor to the recovered grease, may be removed by agitating such petrolic ether solution with a dilute solution of sulfuric acid or its equivalent: and this may be followed by a treatment with magnesium oxid in the form of a dry powder with which the solution is agitated.

\Ye have discovered that in this treatment the settling of the last traces of fullers' earth which remain suspended in the petrolic ether solution of the grease, and which are very difficult to filter, may be much hastened by the addition of about 2 per cent. of alcohol. The addition of this alcohol precipitates the fine clay or fullers earth in the petrolic ether in coarse flocculent form. This feature of precipitating the clay by means of alcohol is a very important one. being comparable with the use of a coagulant such as alum for hastening the settlement of clay in muddy water. So far as we are aware. no coagulant has heretofore been known for clay suspended in petrolic ether. This feature can also be used to advantage in the recovery of the wool grease from wool for the purpose of precipitating any clay or similar matter contained in the wool and which may be extracted with the grease.

After the petrolic ether solution of the grease has been clarified by settling, it is drawn off and the residual fullers earth is given a washing with petrolic ether. The petrolic ether solutions are distilled and the grease thus recovered.

The grease may be freed from odor of petroleum by blowing with air or other gases at a temperature of from 90 degrees to 100 degrees C.

The free fatty acids and dissolved neutral grease are recovered from the ammoniacal alcohol by distilling off the alcohol and ammonia, which may be then used for further operations.

The method herein described possesses many advantages, among which may be mentioned the following:

First. It may be and is conducted at ordinary temperatures.

Second. It does not darken the grease.

Third. The volatile base employed can be recovered by distillation and re-nsed.

Fourth. The fatty acids and the small amount of neutral grease temporarily combined with or dissolved by the base can be recovered without the use of any acid. Heat readily breaks up the combination.

Fifth. Emulsion troubles are entirely done away with, no water being used at any stage, except in washing out ammonia from the petrolic other solution of the grease. For this purpose, but water or acid is used.

Sixth. The process is exceedingly simple, and can be rapidly carried out.

Seventh. The bleaching operations and the precipitation of the fullersearth are greatly facilitated and improved.

Eighth. There are no losses in the process, except such as are caused by imperfect condensation of the volatile solvents.

'e do not desire to limit ourselves to the exact methods. temperatures, or proportions, hereinbefore described, since these may be varied without departing from the spirit and scope of our invention as defined in the appended claims.

By the term petrolic ether as used herein and in the appended claims, we intend to include naphtha, gasolene, and all similar petroleum products having a sutliciently low boiling point. The boiling point should not be sufliciently low to cause loss, and, on the other hand, it should not be sufiiciently high to give undesirable residual products under the conditions of evaporation employed. In practice we have found a boiling point of from degrees to 100 degrees and preferably between degrees and 100 de-' grees C., to give good results.

\Ve claim:

1. In the art of refining wool grease, the method which consists in dissolving the grease in petrolic ether. and then treating the solution with ammonia, substantially as described.

2. In the art of refining wool grease, the method which consists in dissolving the grease in petrolic ether, and then treating the solution with ammoniacal alcohol, substantially as described.

3. In the art of refining wool grease. the method which consists in dissolving the grease at ordinary temperatures and at substantially atmospheric pressure in a neutral solvent containing no chemical reagent, and then treating the solution with an ammonium hydrate liquor, substantially as described.

4. In the art. of refining wool grease, the method which consists in dissolving the grease at ordinary temperatures and at substantially atmospheric pressure in a neutral solvent containing no chemical reagent, and then treating the solution with ammoniacal alcohol, substantially as described.

5. In the art of refining wool grease, the method which consists in dissolving the grease at ordinary temperatures and at substantially atmospheric pressure in a neutral solvent containing no chemical reagent, and then treating the solution with a mixture of ammonium hydrate and alcohol, substantially as described.

6. In the art of refining wool grease, the method which consists 1n dissolving the grease at ordinary temperatures and at substantially atmospheric pressure in a neutral solvent containing no chemical reagent, and then mixing the solution so formed with successive portions of ammoniacal alcohol of different strengths, and drawing off the alcohol liquid containing the free fatty acids after each treatment, substantially as described.

7. In the art of refining wool grease, the method which consists in dissolving the grease in petrolic ether, treating the solution so formed with ammoniacal alcohol, drawing off the alcoholic liquid containing the free fatty acids, and recovering the free fatty acids and dissolved neutral grease therefrom, substantially as described.

8. In the art of refining wool grease, the method which consists in dissolving the grease in petrolic ether, treatin the solution so formed with ammoniacal a cohol, drawing off the alcoholic liquid containing the free fatty acids and some dissolved neutral grease, and recovering such acids and grease from the alcohol by distilling off the alcohol and ammonia. substantially as described.

9. In the art of refining wool grease, the method which consists in dissolving the grease in petrolic ether, treating the solution with ammoniacal alcohol, drawing off the alcoholic liquid containing the fi fatty acids and some dissolved neutral grease, and treating the remaining petrolic ether solution containing neutral wool grease with fullers earth, substantially as described.

10. In the art of treating wool grease, the method which consists in dissolving the grease in petrolic ether, treating the solution with ammoniacal alcohol, drawing off the alcoholic liquid containing the free fatty acids and some dissolved neutral grease, treating the remaining petrolic ether solution containing the neutral wool grease with fullers earth, and completing t e settling of the fullers earth suspended in the petrolic ether solution by the addition of alcohol, substantially as described.

11. In the art of treating wool grease, the method which consists in dissolving the grease in petrolic ether, treating the solution with ammoniacal alcohol, drawing off the alcoholic liquid containing the free fatty acids and some dissolved neutral grease, treating the remaining petrolic ether solution containing the neutral wool grease with fullers earth, completing the settling of the fullers" earth suspended in the petrolic ether solution by the addition of alcohol, and then distilling the petrolic ether solution to recover the grease, substantially as described.

12. Inthe art of refining wool grease, the method which consists in dissolving the grease in a solvent, treating the solution so formed with ammoniacal alcohol, drawing off the alcoholic liquid containing the free fatty acids and some dissolved neutral grease, and recovering such grease, bleaching the grease contained in solution in the original solvent. and then distilling such solution and recovering the grease, substantially as described.

13. In the art of refining wool grease, the method which consists in dissolving the grease in a solvent, treating the solution so formed with ammoniacal alcohol, drawing off the alcoholic liquid containing the free fatty acids and some dissolved neutral grease, recovering such grease, bleaching the grease contained in solution in the original solvent, then distilling such solution and recovering the grease, and finally freeing the grease from petroleum odors, substantially as described.

14. In the art of treating wool grease, the method which consists in forming a petrolic ether solution containing neutral grease only, treating such solution with fullers earth, and precipitating the fullers earth from such solution b the addition of alcohol, substantially as described.

15. In the art of refining wool grease, the method of removing free fatty acids which consists in making a solution of the grease in petrolic ether and agitating it with ammoniacal alcohol, substantially as described.

16. In the art of refining wool grease, the method which consists in forming a solution of the grease in a neutral solvent containing no chemical reagent, and then treating the solution with a volatile base to neutralize the free fatty acids present in the solution, substantially as described.

17. In the art of refining wool grease, the method which consists in forming a solution of the grease in a volatile neutral solvent containing no chemical reagent, then treating the solution with a volatile base, removing the fatty acids from the solution, and then distilling the remainder of the solution and recovering the neutral grease, substantially as described.

18. In the art of treating wool grease, the method which consists in forming a solution of the grease and precipitating the clayey matter originally contained in the grease by the addition of alcohol to the solution, substantially as described.

19. In the art of treating wool rease, the method which consists in disso ving the grease in a solvent, adding absorbent material thereto, and precipitating such material from the solution by the addition of alcohol, substantially as described.

20. In the art of refining wool grease, the method which consists in dissolving the grease in a neutral solvent containing no chemical reagent, then treating the solution with ammoniacal alcohol, and then treating to remove any ammonia remaining in the solution, substantially as described.

21. In the art of refining wool grease, the method which consists in dissolving the grease in a neutral solvent containing no chemical reagent, then treating the solution with aminoniacal alcohol, and then agitating the solution with a dilute solution of sul furic acid or its equivalent to remove any contained ammonia, substantially as described.

In testimony whereof, we have hereunto set our hands.

JAMES O. HANDY. ROBERT M. ISHAM. Witne W. C. LYON, H. M. ConwIN.

grease in a neutral solvent containing no chemical reagent, then treating the solution with ammoniacal alcohol, and then agitating the solution with a dilute solution of sulfuric acid or its equivalent to remove any contained ammonia, substantially as described.

orrection in Letters Patent No.1,194,013.

In testimony whereof, we have hereunto WV. C. LYON,- H. M. ConwiN.

It is hereby certified that in Letters Patent No. 1,194,013 granted August 8, 1916, upon the application of James 0. Handy and Robert M. Ishain, of Pitts- *burgh, Pennsylvania, for an improvement in Methods of Refining Wool-Grease? an error appears in the printed specification requiring correction as follows: Page 3, line 118, claim 19, for the word absorbent read adsorbent; and that the said Letters 1 itent should be read with this correction therein that the same may conform to the record of the case in the Patent Oflice.

Signedand sealed this 21st day of November, A. D, 1916.

F. W. H, CLAY, Actino Commissioner of Patents.

[SEAL-l orrection in Letters Patent No. 1,194,013.

It is hereby certified that in Letters Patent No. 1,194,013, granted August 8,

0. Handy and Robert M. Isharh, of Pittsburgh, Pennsylvania, for an improvement in Methods of Refining Wool-Grease, an error appears in the printed specification requiring correction as follows: Page 3, line 118, claim 19, for the Word absorbent read adsorbent; and that the said Letters 1 itent should be read with this correction therein that the same may conform to the record of the case in the Patent Office.

Signed and sealed this 21st day of November,A. D., 1916.

F. W. H. CLAY,

Acting Commisaimwr of Patents.

1916, upon the application of James [SEAL]