US2665282A - Treatment of wool grease - Google Patents

Description

Patented Jan. 5, 1954 TREATMENT OF WooL GREASE John P. Stanley, Amsterdam, N. Y., assignor to Mohawk Carpet Mills, Inc.',

Amsterdam, N. Y.,

a corporation of New York No Drawing. Application March 22, 1950,

Serial No. 151,322

7 Claims.

This invention relates to the treatment of lanolin or wool grease and the production of a product having improved emulsifying properties.

More particularly, the invention relates to an improved process in which lanolin or wool grease is subjected to a limited and partial oxidation by treatment with chemical oxidizing agents such as sodium chlorite and sulfuric acid, etc., to produce products having improved emulsifying properties.

The usual methods of emulsifying lanolin or wool grease involve the use of added soaps or other emulsifying agents, or dissolving in a solvent and then effecting the emulsification with a soap or emulsifying agent.

I have found that lanolin or wool grease can be converted into a readily emulsifiable product by treatment with oxidizing agents and effecting a limited and partial oxidation thereof, and by adding a small amount of alkali to the oxidized product.

The oxidation of the lanolin or wool grease is effected by chemical oxidizing agents such as a mixture-of sodium chlorite and sulfuric'acid.

The invention Will be further illustrated by the following examples:

Example I .l kilos of crude (neutral) lanolin or 'wool grease are placed in a closed vessel provided with heating means and a stirrer and there is added 1.5 liters of 10% tion-with stirring followed by the addition of 0.2 liter of 50% sulfuric acid. The whole mixture is then well stirred and allowed to stand about 16 hours at room temperature (21-24 C.) and then heated at 100 C. for about 1 hours. mixture is then washed with water by'adding about twice as much water as there is of the mixture with stirring and heating to above the melting point and then cooling, after which the water is drawn off. This washing treatment is repeated three times. The resulting washed product is then heated to the melting point. Approximately 25 kilos of water containing sufficient potassium hydroxide to make the resulting mixture with the wool grease product alkaline to litmus is heated to approximately the same temperature as the melting wool grease product and then poured into the product with thorough stirring. This results in a smooth emulsion of the oil-in-water type.

The amount of sodium chlorite and of sulfuric acid can be varied somewhat and products varying somewhat in their emulsifying properties obtained. Thus, from about 0.04 part of sodium chlorite for each 10 parts of wool grease .up to 2 parts of sodium chlorite for each 10 parts of sodium chlorite solu- 4 The'- wool grease have been tried and the best results were obtained with the larger quantities. Similarly, various quantities of sulfuric acid were tried from about 0.1 part of sulfuric acid for 10 parts of wool grease to 0.25 part of sulfuric acid for 10 parts of wool grease, depending upon the amount of sodium chlorite used and usually having enough acid present so that the reaction took place in an acid medium. Other acids, e. g., hydrochloric acid, can be used instead of sulfuric acid.

The process can be carried out at different temperatures and for different periods of time, varying from room temperature to around C. and from around 16 hours to hour for the chlorite treatment.

Example II.-10 kilos of wool grease are treated with 6.5 liters of 10% sodium chlorite solution which are stirred into the wool grease and then 0.35 liter of l 50% sulfuric acid are added and stirred in and thereaction is allowed to proceed at room temperature (2l-24= C.) for 1 hour with intermittent stirring. The vessel is heated up to 100 C. for 15 minutes after which the product is washed three times with water. The product is then melted at a temperature of 40*50 C. and 25 liters of 1% sodium carbonate solution previously heated to 40-50 C. are added and stirred in, with resulting formation of a good emulsion.

Various kinds and strengths of alkali were tried and it was found that in general there should be sufiicient alkali present to make the whole product alkaline. Thus, potassium hydroxide, sodium hydroxide, sodium carbonate, ammonium hydroxide; sodium borate, and triethanolamine were all used as additions to the product resulting from the treatment of the wool grease or lanolin with sodium chlorite and acid. A 1% solution of sodiumcarbonate is advantageously used.

In the processes of the above examples chlorine dioxide is formed as an oxidizing agent. When chlorine dioxide gas is used or is formed during the reaction a closed vessel is advantageously used.

The action of the limited and partial oxidation treatment of the lanolin or wool grease is to increase substantially the free acidity. Thus, when washed U. S. P. lanolin having an initial acidity of oleic acid of 0.98 was treated in a manner similar to that indicated in Example II above the oxidized product had an acid value of about 1.8%. When treated again with the same quantities of sodium chlorite and sulfuric acid the acidity increased to about 5.75 A similar treatment with an increased amount of sodium chlorite equal to one-fifth the weight of the wool grease and with twice the amount of sulfuric acid used in Example II gave a product having an acid value of about 3.97%. All of these products were readily emulsifiable, those with higher acidities having somewhat better emulsifying properties. Other changes, other than the increase in acidity, also appear to be brought about by the limited and partial oxidation. A slight decrease has been observed in the saponification number of the treated product as compared with the product before treatment. The presence of the increased amount of free acids produced by the oxidation treatment results in the formation of salts or soaps with the added alkali and gives a product having improved emulsifying properties.

In the process illustrated by the above examples an emulsion is usually formed in the treatment as the chlorite and acid are in aqueous solution and are mixed in with the lanolin, and the reaction product was washed with water. The process can be somewhat improved by breaking any emulsion that remains at the end of the process prior to washing to remove the inorganic acids and salts. One method of doing this is to dissolve the product in a solvent such as ethyl ether, ethylene dichloride or chloroform, then washing the solution with water and subsequently separating the solution and evaporating the solvent and drying the product. A centrifugal method of breaking or separating the emulsion can also be used.

The oxidized lanolin or wool grease product resulting from the limited and partial oxidation treatment contains an increased amount of free acids resulting from the oxidation treatment and is an improved emulsifiable product. It can readily be converted into an emulsion by the addition of water containing sufficient alkali to make the resulting product slightly alkaline although in some cases an excess of alkali, e. g., sodium carbonate, may be present.

It is one advantage of the new lanolin or wool grease product, resulting from treatment with oxidizing agents, that the products are emulsifiable without the addition of soaps or emulsifying agents, and that emulsions can be prepared therefrom simply by the addition of weak alkaline solutions. As a result the emulsifying process is more flexible and adjustments can readily be made in the solids content of the emulsions. Another important advantage of the product is that it is more easily saponified when it is desired to separate the acids and alcohols contained in the oxidized products for the production, e. g'., of cholesterol and wool fat acids including acids formed by the partial oxidation treatment.

Iclaim: I

1. The method of treating lanolin or wool grease to improve the emulsification properties thereof which comprises subjecting the same to a limited and partial oxidation treatment with an aqueous acid chlorite oxidizing agent and continuing such oxidation treatment until there is an increase of from about 9.82% to 4.77% in the free acidity and to give an oxidized product which, after washing with water, forms emulsions on the addition of weak aqueous alkaline solutions.

2. The process according to claim 1 in which the treatment is with a mixture of a solution of sodium chlorite and of sulfuric acid.

3. The method according to claim 1 in which the oxidized product is Washed with water.

4. The process according to claim 1 in which the product after washing is emulsified with a dilute alkaline solution sufficient in amount to give an emulsion with an alkaline reaction.

5. The process according to claim 1 in which the product after washing is emulsified and saponified with an alkaline solution to separate the alcohols from the acids.

6. The method of treating lanolin or wool grease to improve the emulsification properties thereof which comprises subjecting the same to a limited and partial oxidation treatment with an aqueous solution of sodium chlorite and sulfuric acid, continuing such oxidation treatment to effect an increase of from about 0.82% to 4.77% in the free acidity, washing the resulting product with Water, and preparing an emulsion therefrom by the addition of a dilute alkaline solution sufficient in amount to give an emulsion with an alkaline reaction.

7. An oxidized lanolin or wool grease product containing from about 1.8% to 5.75% of acids resulting from a limited and partial oxidation treatment thereof with an aqueous acid chlorite solution, said product forming oil-in-water emulsions on the addition thereto of a dilute aqueous alkaline solution.

JOHN P. STANLEY.

References Cited in the file of this patent UNITED STATES PATENTS Number Name Date 2,473,930 Woodward June 21, 1949 2,481,463 Woodward Sept. 6, 1949 FOREIGN PATENTS Number Country Date 214,937 Germany of 1906 386,715 Great Britain of 1933 OTHER REFERENCES Chem. Abst. 35-6348

Claims (1)

1. THE METHOD OF TREATING LANOLIN OR WOOL GREASE TO IMPROVE THE EMULSIFICATION PROPERTIES THEREOF WHICH COMPRISES SUBJECTING THE SAME TO A LIMITED AND PARTIAL OXIDATION TREATMENT WITH AN AQUEOUS ACID CHLORITE OXIDIZING AGENT AND CONTINUING SUCH OXIDATION TREATMENT UNTIL THERE IS AN INCREASE OF FROM ABOUT 0.82% TO 4.77% IN THE FREE ACIDITY AND TO GIVE AN OXIDIZED PRODUCT WHICH, AFTER WASHING WITH WATER, FORMS EMULSIONS ON THE ADDITION OF WEAK AQUEOUS ALKALINE SOLUTIONS.