US2150732A - Method of treating vegetable oils and product obtained thereby - Google Patents

Description

METHOD OF TREATING VEGETABLE OILS AND PRODUCT OBTAINED THEREBY Original Filed Feb. 14-, 1935 Patented Mar. l4, 1939 UNITED STATES METHOD OF TREATING VEGETABLE OILS AND PRODUCT OBTAINED THEREBY Benjamin H. Thurman, Bronxville, N. Y., assignor to Refining, Ina, Reno, Nev., a. corporation or Nevada Application February 14, 1935, Serial No. 6,446 Renewed March 31, 1937 52 Claims.

This invention relates to the recovery of valuable constituents from vegetable oils and the products thereby obtained, as well as the utilization 01 such products. It relates more particu- 5 larly to the treatment of cottonseed oil for this purpose, but is not restricted to this oil, as other vegetable oils, such assoya bean, rape seed, cocoanut, corn, linseed, etc., from which lecithin-like bodies or phosphatides may beobtained, may be used. It is well known that cottonseed oil that has been obtained by pressing the seed contains only a small percentage, that is, less than about five percent by weight of such phosphatides.

This application is a continuation in part of my applications, Serial No. 6%,137, filed November 23, 1932, and Serial No. 676,932, filed June 21, 1933.

Heretofore attempts have been made to obtain phosphatides, sometimes called vegetable lecithin from soya beans or other seeds with a solvent or solvents. This has not proven satisfactory because it is expensive and also because some of the oil is dissolved from the beans or seeds and must be removed to prevent the same from contaminating the phosphatides. It has proven to be very difllcult, if not impossible, to remove a sufilcient amount of the oil and other impurities from the phosphatides to render the same'tasteless and odorless and free from the tendency to become rancid. In addition, the solvent or solvents used are expensive and must be distilled on to free the lecithin. I

Materials referred to as "impurities have heretofore been removed from crude fatty oils, ineluding cotton seed oils, by hydrating the impurities to render them insoluble in the oil and then removing them from the oil so that the oil can be more readily refined by treating the same with alkali. The impurities that were rendered insoluble in this way and removed from the oil have been discarded as waste material.

By the present invention compounds that are apparently phosphatides, or so-called vegetable lecithin, can be recovered in large amounts from vegetable oils in a very convenient and economical manner without requiring complicated apparatus or a high degree of skill and experience,

refine it and these removed materials can be readily refined so as to leave substantially tasteless and odorless phosphatides that do not become rancid for a long time or undergo rapid oxidation even at considerably elevated temperatures. The claims hereof accordingly are intended to be limited to the improvement of separating materials containing phosphatides from vegetable oils before the same have been treated with an alkali in sufllcient quantities to substantially saponliy the free fatty acids of the oil, thereby to refine the same; it constitutes no part of my invention to continuously effect saponiflcation of the free fatty acids to remove the same from the oils. In this way a supply of phosphatides that are substantially free from deleterious agents or impurities, and are very useful in the arts are economically obtained.

This invention will be described in detail in connection with the recovery of the valuable materials from cottonseed oil by way of an illustrative example, although proportions, temperatures and time of treatment may be varied over wide ranges and a variety of agents may be utilized in the process, and other vegetable oils containing phosphatides may be treated in a similar manner.

In carrying out this invention cottonseed oil, that has been obtained in the well known way by crushing the seed, removing the husks and pressing the residue, thus forming the cake and obtaining the oil, is treated, preferably, although not necessarily, while the oil is fresh with a reagent which will precipitate phosphatides and possibly other products that are in solution or colloidal suspension in the oil. The treatment with the reagent also probably causes chemical reactions to' take place, the nature of which is not thoroughly understood. The precipitated material may be removed or separated from the oil by settling, filtering or centrifuging. The separated material may be further purified so as to have it in better condition for use or sale. The oil may of course be filtered before treating with the reagent so as to remove fibrous material and other solids that may be present. A large variety of reagents may be added to the oil for the purpose of precipitating the phosphatides. Among the reagents that may be used may be mentioned water, alcohol and electrolytes, such .as aqueous solutions of acids, alkalies and salts, for example. In fact, extensive investigations indicate that either water or any electrolyte is satisfactory for this purpose. By "electrolyte is meant a solution of an acid or a salt in water of such a nature that it will not react materially with the oil or damage it. It is preferable to agitate the mixture for a few minutes after the reagent has been added, after which the precipitate is removed from the oil in any convenient way as by settling and decanting, filtering or centrifuging. The temperature may be from room temperature, say about 20 C. or lower, to 110 C., or higher.

When water alone is used to precipitate phosphatides from cotton seed oil only about 1 to 10% by volume of water is needed. The amount of water needed will vary to some extent with the particular oil and the age thereof, 2% to 5% being sufiicient for many vegetable oils. The desired amount of the reagent that is needed, whether water, or other suitable reagent for pericipitating the phosphatides, can be ascertained by tests with samples of the oil. The amount. of the reagent that will ordinarily be used for this purpose is usually preferably the amount which will cause the maximum amount of phosphatides to be precipitated from the oil.

The reagent should be intimately mixed with the vegetable oil before the precipitate is separated, as mentioned above. The mixture may be by agitation, as mentioned above, or the oil may be passed through a pipe into the middle portion of which a smaller pipe with a closed end projects, this smaller pipe being provided with perforations near its end and surrounded with a porous cloth or the like and used for introducing the reagent into the oil and intimately distributing it therein, or otherwise. When water is to be used water itself or steam may be introduced into the oil. When steam is used it appears to act as a coagulating agent in the removal of the phosphatides as a precipitate from the cotton seed oil.

It has been found that the phosphatides can be removed from the vegetable oils in a continuous process by introducing the water or electrolyte into a flowing stream of the oil that is passing through a curved pipe, for example, where the cross section or the change in direction, or both, are such that an intimate mixture of the water or electrolyte with the vegetable oil will be effected.

A convenient arrangement of apparatus for carrying out the process in a continuous manner is somewhat diagrammatically illustrated in the accompanying drawing in which parts are shown in section.

In the drawing reference character I indicates a storage tank for the vegetable oil and reference character 2 indicates a similar tank for the water or other reagent or electrolyte to be mixed with the oil. A valved pipe 3 leads from the tank I to the pump 4 from which a pipe 5 leads to the mixer 6. A valved pipe 8 leads from the tank 2 to the pump 8 from which a pipe 9 leads to the mixer 6. A pipe l0 leads from the mixer 6 to a coil pipe I I that may be located in a housing l2. The lower end of the coil H opens into a centrifugal separator l3 or other device for separating solids from liquids.

In the operation of the process with an arrangement of apparatus such as that shown in the drawing, the pump 4 forces oil from the tank I and the pump 8 forces water or an electrolyte from-the tank 2 into the mixer 6, the proportions of the two liquids being regulated by the valves in the pipes 3 and l. The mixture passes from the mixer 6 through the coil or pipe ll so that the mixture does not stratify into layers, but keeps well mixed, or the change in direction of travel of the mixture through this coil causes the two liquids to become intimately mixed with each other if they should not'be sufficiently mixed before they reach it.

If desired, the housing llor the coil ll may be heated in any convenient way to facilitate the flow of the mixture through the coil, or the oil in the tank I may be heated to make the same less viscous, thereby facilitating a more intimate mixture of the oil and reagent or electrolyte as they become mixed in the mixer 6.

The pipe may be in the form of a coil, as shown by the coil II, or it may be bent into other shapes. This portion of the pipe is preferably made with bends or sharp turns in it so that if the mixture is not well mixed before it reaches this portion it will become well mixed, or if the liquids have been well mixed before they reach this portion they will remain well, mixed without any tendency for the same to stratify or separate into layers of the different constituents.

There are certain advantages in carrying out this process in a continuous manner, as can be done, for example, by an arrangement of apparatus illustrated in the drawing. One of the advantages of the continuous process as compared to a batch process is that the substances that are to be precipitated from the oil do not become segregated as they would if a batch were made up of the oil and reagent or electrolyte, stirred, until the proper effect is produced, and then permitted to stand for a little while. In the case of the batch process the tendency of the material to settle out would interfere with the operation in the centrifugal separator, whereas the uniform mixture with the even dispersion of the particles of solid material throughout the liquid portion in the continuous process as the mixture leaves the pipe or coil It makes it possible to effect a quick and satisfactory separation of the constituents in the centrifugal machine l3.

It has usually been found that more satisfactory results and somewhat higher yields are obtained when dilute acids are used as the precipitating media instead of water alone. A 10% boric acid solution in water has proven to be especially suitable. Only about 1% of this solution compared to the volume of oil treated is ordinarily needed. Other dilute acids, such as sulphuric, phosphoric and acetic are also suitable, as well as salt solutions, such as sodium sulphate and bisulfate, sodium borate, etc., and dilute alka- 1i solutions, such as trisodium phosphate and triethanolamine and other electrolytes for precipitating the valuable materials or phosphatides from cotton seed oil.

In treating the oil with the reagent to precipitate phosphatides the proportions, temperatures, and time of treatment may be varied over wide ranges, depending to some extent upon'the particular oil that is being treated and also to some extent upon the material that is used as the reagent.

By testing with a second reagent the oil that has been treated for a given time at a particular temperature, it can be ascertained whether the first treatment with the reagent has been suflicient to remove the desired amount of phosphatides.

After the precipitates have been separated from the oil, as described above, they maybe purified to remove extraneous or deleterious matter, leaving a, purified residue that is very valuable in the arts for many useful purposes. The solid content of the precipitate obtained from cotton seed oil contains about 60 or of the valuable phosphatides from which a large portion or substantially all of the remaining solids or dele-' terious matter can be removed. Such remaining purified phosphatides are of 'such a character that they do not have an objectionable taste or odor and do not become rancid for a long time even when exposed to air, or certain ingredients which appear to aid in preserving the phosphatides may have been precipitated from the oil with the phosphatides and are not removed during the purification step.

Another method of purifying the precipitated phosphatides is to wash the phosphatides in acetone, since the impurities are for the most part soluble in acetone. The phosphatides may be dissolved in ether and another oil, such as cocoanut oil, may be added, and then the ether evaporated. The precipitated phosphatides may also be advantageously washed with hot alcohol before dissolving in ether, thus removing certain impurities that are soluble in hot alcohol.

Instead of first precipitating the phosphatides from the oil and afterwards washing them to purify them, the oil may be filtered'or otherwise treated to remove solids, and then treated as described above to precipitate the phosphatides, whereupon they will be sufliciently pure to make them available for use in the arts. They may be dried before being used.

It has been found that often when water alone is used for washing the phosphatides or precipitates from the oil a very tenacious emulsion is formed so that washing the precipitates with water alone is sometimes impractical. It has been found, however, that when sodium chloride is added troubles due to formation of emulsions are avoided. A small amount of this salt may be added to the emulsion to break it or an aqueous sodium chloride solution may be used instead of the water for washing the precipitates. Salt, NaCl, to the extent of about 10% of the water has been found to be satisfactory. The use of the salt either breaks the emulsion or prevents the same from being formed and the aqueous salt solution apparently has a solvent action on some of the globulin and 'albuminoid substances so that they are removed during the washing step. Also, the remaining insoluble phosphatides are left in small particles. The phosphatides maybe washed repeatedly with water containing salt until the reagent which was used for precipitating the phosphatides from the oil is removed. This washing also removes impurities or deleterious material. The phosphatides or remaining product may be dried.- The drying is preferably done in a vacuum with a temperature not exceeding about 70 C. The dried product may be washed with acetone to remove acetone soluble materials, such as fatty acids, coloring materials and small amounts of other undesirable substances. The remaining acetone may be distilled off while the air is excluded from the product. When the purified dried material is obtained from cotton seed oil it is yellow and is in the form of a powder.

When the precipitate has been washed with salt water to remove impurities or objectionable material and the product has been dried, whatever salt may remain can be removed by washing with dilute acid, such as hydrochloric acid, the pH of the water being kept about 2.5 to prevent re-emulsificatlon of the phosphatide particles with the wash water. t

It has also been found that water can be used for washing the phosphatides without having salt be centrifuged or filtered out.

dissolved in it, provided the pH of the water is kept sufllciently low, say about pH 3 to prevent emulsification. Chlorine ions appear to be particularly advantageous in preventing emulsification, although other acids and acid salts, such as tartaric, citric, sulphuric acidsand sodium salts and sodium acid salts, for example, which will lower the pH of the solution, can be used. Calcium chloride or aluminum sulphate may also be' used. However, hydrochloric acid has thus far been found to be the most satisfactory for this purpose.

The purified dry product may be dissolved in a non-solidifying oil, such as sunflower oil, sesame oil, or other vegetable oils in their natural state, or partially or completely hydrogenated and the substances that are insoluble in these oils may The percentage of oils used for dissolving the product may be 40% or more of ,the weight of the product that is dissolved in the oil.

The purified phosphatides or vegetable lecithin obtained from vegetable oils in accordance with this invention are useful for many purposes, among which may be mentioned: (a) a. very small amount thereof added to chocolate coating materials containing chocolate, sugar and fat will materially reduce their viscosity, thus making them more suitable for making coatings; (b) one quarter to one-half per cent thereof added to margarine prevents the same from foaming or spattering when heated, thus permitting food such as eggs to be browned when fried therein; one twentieth to one per cent thereof added to fats, such as cocoanut oil plastics, enables them to absorb water more easily and readily; (d) a small quantity added to fats used in making caramels enhances the qualities of the caramel and makes itmore palatable.

Some of the characteristics which distinguish the phosphatides or product obtained, as described above, from cotton seed oil, from similar products are as follows:

(a) This product is yellowish in color and contains approximately the same percentage of phosphorus, namely about 2.6% calculated on a dry basis, as the precipitate that precipitates out of the oil after it has been allowed to stand for a long time without the addition of a precipitating reagent.

(b) The iodine number of the purified product is approximately 60, while the iodine number of the purest previously known vegetable lecithin products is about 90.

(0) Fatty acids obtained from this purified product or phosphatides have an iodine number of about 95 while the iodine number of cotton seed oil is about 108 and the iodine number of soya bean oil, as well as the fatty acids from lecithin obtained therefrom, is about 125. The low iodine number of the product of this invention and the fatty acids obtained from its probably explains, at least in part, why the product of this application will keep such a long time or has very little tendency to absorb air and become rancid.

(d) The product or phosphatides of this invention may be dissolved in high boiling oils, such as sunflower seed oil and heated to 440 F. without changing color very much and without having a very noticeable amount of objectionable black color and a very nauseating odor and un- Iii) half oi 1% thereof added to vegetable oils greatlydecreases the tendency of these oils to become rancid even attemperatures up to 150 F. or

higher over an extended period of time; about 1% or less thereof added to dressings, such as mayonnaise, materially increases the keeping qualities of the same and prevents or greatly retards rancidity; less than 1% added to deep frying oils or fats prevents or greatly retards rancidity and acquisition of bad flavors or odors even at temperatures somewhat above 400 F.; and a small amount thereof added to fats used. in making caramels improves the quality of the caramels without imparting any objectionable taste.

Even the raw or unpurifled phosphatides obtained from cotton seed oil in accordance with this invention are useful for certain purposes. The product may be dried in a vacuum and when so dried it will not deteriorate or putrify in a long time, even when water is used as the precipitating agent. When boric acid is used for recovering the product from cotton seed oil, as described above, the product will keep indefinitely with or without drying and without further treatment. The product will keep after the boric acid has been neutralized with caustic soda and washed out with salt water and the product is dried. The product thus obtained, either purified or unpurified, may be used as an emulsifier. For example, itmay be used for making asphalt emulsions for impregnating wood and also for emulsifying oils to be used in the leather industry as an aid in fat-liquoring and for making paints and varnishes. In places where the yellow color would be' objectionable the phosphatides can be bleached with hydrogen peroxide or sulphur dioxide.

The phosphatides extracted from cotton seed oil in accordance with this invention differ considerably from other phosphatides and also from phosphatides extracted from cotton seed oil that has been obtained from cotton seed by solvent extraction. For example, when cotton seed oil is extracted from cotton seed by a solvent consisting of two parts alcohol and three parts benzol and the solvent is evaporated 01f, the oil contains about ten times as much gossypol as cotton seed oil that is obtained by hot-pressing the cotton seed. The crude material obtained from cotton seed oil, that has been pressed from the cotton seed, in accordance with the present invention contains about 2.9% of reducing sugar while that obtained by treating an alcohol-benzol solvent extract of the cotton seed with steam to obtain the material contains about 31% of reducing sugar. Some of the sugar in each material exists in combination with other components, the per-- centage of the bound sugar in the former material being about 2.6% and about 17.2% in the latter.

The phosphatides obtained from cotton seed oil in accordance with this invention differin a very important respect from phosphatides obtained from soya bean 011, for example, in that they are entirely free from linolenic acid.

It has been found that mayonnaise containing soya bean oil will remain fresh for a few days but will develop thereafter a charac .erlstic soya bean oil odor and flavor but when .3% of the product or phosphatides obtained from cottonseed oil by this invention is added, this product acts as an antioxidant or at least prevents development of the characteristic objectionable odor and flavor from the soya bean oil. This may possibly be due to the prevention of the action of enzymes or bacteria in the soya bean oil used in making mayonnaise dressing. When about 0.1% of this product is added to butter it prevents formation of strong odors even when the butter is e to the atmosphere for a long time and it also prevents water from leaking out of the butter, probably because it is a good emulsifying agent for the butter. This cotton seed 011 product is also valuable as an apparent anti-oxidant in the manufacture of rubber, as well as an excellent anti-oxidant when put in linseed oil varnish that is to be used for painting rubber goods. The addition of even less than 1% of the product to fats or oils that are used for frying vegetable products greatly reduces the tendency of these fats or oils to split and form products that are characteristic of overheated fats, thus imparting substances to the i'ood products that would cause them to become rancid. Food products, such as potato chips-that have large surfaces, are especially prone to become rancid very rapidly by oxidation. The use of the product, that is obtained from cotton seed oil by this invention, in fats or oils for frying such vegetables protects the products and permits the same fatty oil to be used repeatedly for frying them.

I claim:

1. The process of recovering .phosphatides from vegetable oil which contains less than 5% of phosphatides, which comprises treating the oil with a reagent which will precipitate phosphatides, separating them from the oil, and purifying them.

2. The process of recovering phosphatides from vegetable oil which contains less than 5% of phosphatides, which comprises treating the oil with a reagent containing water which will precipitate phosphatides, separating them from the oil, and purifying them.

3. The process of recovering phosphatides from vegetable oil which contains less than 5% of phosphatides, which comprises treating the oil with a reagent which will precipitate phosphatides, separating them from the oil, washing them with water, and drying them.

4. The process of recovering phosphatides from vegetable oil which contains less than 5% of phosphatides, which comprises treating the oil with a reagent which will precipitate phosphatides, separating them from the oil, dissolving the phosphatides, and evaporating the solvent.

5. The process of recovering phosphatides from vegetable oil which contains less than 5% of phosphatides, which comprises filtering the oil, treating it with a reagent that will precipitate phosphatides but which will not eflect substantial saponification, and separating the phosphatides from the oil.

6. The process of recovering phosphatides from vegetable oil which contains less than 5% oil phosphatides, which comprises treating the oil with a solution of an electrolyte which will precipitate phosphatides, separating them from the oil, and purifying them.

7. The process of recovering phosphatides from vegetable oil which contains less than 5% of phosphatides, which comprises treating the oil with 2 to 5% of water which will precipitate phosphatides, separating them from the oil, and purifying them.

8. The process of recovering phosphatides from crude vegetable oil containing fatty acid and various other impurities and less than 5% of phosphatides, which comprises precipitating phosphatides from said oil by adding a reagent that will precipitate phosphatides from the oil, and washing said precipitated phosphatides to remove water soluble impurities therefrom.

9. The process of recovering phosphatides from crude vegetable oil containing fatty acid and various other impurities and less than 5% of phosphatides, which comprises mixing sufllcient water with said crude oil toform a precipitate,

separating the precipitate from the oil and treating said precipitate in such a manner as to separate impurities from the precipitated phosphatides.

10. The process of recovering phosphatides from crude vegetable oil containing fatty acid and various other impurities and less than 5% of phosphatides, which comprises mixing a sufficient amount of an electrolyte with said crude oil to form a precipitate, separating the precipitate from the oil, and treating said precipitate in such a manner as to separate impurities from the precipitated phosphatides.

11. The process of recovering phosphatides from crude vegetable oil containing fatty acid and various other impurities and less than 5% of phosphatides, which comprises mixing a sumcient amount of an electrolyte with said crude oil to form a precipitate, separating the precipitate from the oil, and washing said precipitate with -water to remove water soluble material therefrom and leave phosphatides.

12. Substantially tasteless and odorless vegetable phosphatides in the form of a powder having a yellow color and containing about 2.6% of phosphorus.

13. Substantially tasteless and odorless dried vegetable phosphatides in the form of a yellow powder having an iodine number about 60.

14. Vegetable material composed of substantially pure phosphatides in the form of a yellow powder and being capable of being heated to 440 F. in oil without undergoing an objectionable amount of oxidation.

15. The process 01' recovering phosphatides from cotton seed oil, which comprises adding a reagent to the crude oil which will form a precipitate containing phosphatides, separating said precipitate from the oil and washing it with a sodium chloride solution to remove impurities from the phosphatides.

16. The process of recovering phosphatides from cotton seed oil, which comprises adding a reagent to the crude oil which will form a, precipitate containing phosphatides, separating said precipitate from the oil and washing it with water to which about of sodium chloride has cipitate containing phosphatides. separating said precipitate from the oil, treating it to remove impurities from the phosphatides, drying the residue at a low temperature, and washing it with acetone.

19. Substantially tasteless and odorless cotton seed oil phosphatides in the. form of a powder having a yellow color and containing less than 3% of bound sugar.

20. Substantially tasteless and odorless vegetable phosphatides in the form of a powder haveflect substantial saponiflcation, maintaining the oil out-of contact with the atmosphere during said mixing, and continuously centrifugally separating said materials from said 011.

22. A continuous process of separating materials containing phosphatides from vegetable oils.

said mixing, flowing the mixture through an v elongated passageway of restricted cross-section. and thereafter continuously centrifugally separating said materials from said oil.

will precipitate materials containing phosphai tides from the oil but which will not effect substantial saponification, mixing said 011 and reagent in said zone and passing said mixture through an elongated passageway of restricted cross-section, maintaining said mixture at an elevated temperature during its passage through said passageway to reduce the viscosity of said oil, and thereafter continuously centrifugaliy separating the heated mixture so as to separate said materials from said oil.

24. A continuous process of separating materials containing phosphatides from vegetable oils containing less than 5% of phosphatides, which comprises forcing to a mixing zone separate proportioned streams of oil and a reagent which will precipitate materials containing phosphatides from the oil but which will not effect substantial saponiflcation, mixing said oil and reagent in said zone and passing said mixture through an elongated passageway of restricted cross-section. maintaining said mixture at an elevated temperature during its passage through said passageway to reduce the viscosity of said 011, maintaining said'oil and reagent out of contact with the atmosphere during said mixing and passage through said passageway, and thereafter continuously centrifugally separating the, heated mixture so as to separate said materials from said 011.

25. A continuous process of separating materials containing phosphatides from vegetable ols containing less than 5% of phosphatides, which comprises continuously mixing with the oil a reagent which will precipitate materials containing phosphatides from the oil but which will not effect substantial saponification, promptly flowing the mixture, before the precipitated materials have become segregated, through an elongated passageway of restricted cross-section in order to provide an-even dispersion of the precipitated particles, maintaining the mixture at an elevated temperature during its passage through said passageway, and thereafter continuously centrifugally separating the materials from said oil.

26. In the art of obtaining phosphatides from expressed oils having less than 5% of said phosphatides, the step which comprises precipitatingsuch phosphatides without deterioration thereto and thereafter separating the precipitated phosphatides from the oil.

27. A continuous process of separating materials containing phosphatides from vegetable oils containing less than 5% of phosphatides which comprises continuously mixing the oil with a reagent which will precipitate materials containing phosphatides from the 011 without substantial reaction with and damage to the oil and free fatty acid, and thereafter continuously centrifugally separating said materials from the oil.

28. A continuous process of separating materials containing phosphatides from vegetable oils containing less than 5% of phosphatides which comprises the steps of mixing the oil with a precipitating reagent for said materials in the presence of suflicient elevated temperature to facilitate precipitation and promptly, before substantial attack upon the oil or free fatty acids, centrifugally separating the precipitated material from the oil.

29. A continuous process of treating expressed oils containing gums of a nature having phosphatidic materials therein which comprises the steps of continuously admixing the expressed oils with water as a precipitating reagent, limiting the duration of contact of the reagent and oil for such a relatively few .minutes as will prevent injury to the oil during its continuous flow through the system and promptly thereafter separating the precipitated gums from the oil.

30. A quick and continuous process for degumming expressed vegetable oils containing phosphatides which comprises the steps of continuously mixing with the oils, during their continuous flow, a precipitating reagent for the gums containing said phosphatides and which constitutes a preservative for the phosphatides and promptly and continuously, before injury to the phosphatides or to the oil efiecting the separation of the phosphatides therefrom.

31. A continuous process for degumming expressed vegetable oils containing phosphatides which comprises the steps of continuously mix,- ing the oils with a precipitating reagent for the gums containing said phosphatides in the form of a solution suificient to substantially completely precipitate the gums and to thereby condition the oil for use at elevated temperatures without discoloration, or for subsequent refining, but insufiicient to materially attack the free fatty acid or the oil and continuously advancing as a stream the mixture containing the precipitated gums to a separating zone and there continuously removing the thus precipitated materials from the oil.

32. A continuous process for separating gums containing phosphatides from expressed vegetablesoils which comprises the steps of injecting steam into a flowing stream of said oils to coagulate said gums and promptly separating the coagulated materials from the oil.

83. A continuous process for removing gums including phosphatides from expressed vegetable oils which comprises the step of preheating the oil prior to admixture therewith of an aqueous precipitating reagent, thereby to obtain an intimate admixture of the oil and reagent, said reagent being in sufficient concentration to substantially completely precipitate said materials without substantial attack upon the free fatty acid and thereafter promptly centri ugally separating the preciptated gums from the oil.

34. Lecithin obtained from expressed oils and being relatively free of naturally occurring free sugar.

35. Lecithin obtained from expressed oils and being characterized by having not more than substantially 2.9% of naturally occurring free sugar.'

36. A stable, non-fermenting, water containing vegetable lecithin mixture characterized by the incorporation therein of a preserving agent, said preserving agent comprising boric acid.

37. A stable, non-fermenting, water containing vegetable lecithin mixture, said mixture being the reaction product of lecithin, oil and water and a reacting substance of a character incapable of injury to the lecithin and including a. preserving agent.

38. Vegetable lecithin obtained from vegetable oils and having a preservative thoroughly dispersed therein during the precipitation of the lecithin from the oil and constituting a preservative against fermentation.

39. Phosphatides obtained from expressed cottonseed oils characterized by the substantial freedom of gossypol therefrom and being relatively free of naturally occurring free sugar.

40. As a composition of matter, vegetable lecithin having substantial quantities of absorbed water whereby said product is miscible with water.

41. As a composition of matter, vegetable lecithin having substantial quantities of absorbed water and a preservative.

42. The process of continuously producing vegetable lecithin containing absorbed water comprising the steps of' subjecting expressed vegetable oils to precipitation with water as a precipitating reagent and removing the precipitated lecithin with its absorbed water from said oil.

43. The process of separating gums containing phosphatides from fatty oils which comprises the steps of mixing, in stream flow, the oil with a precipitating reagent of a character and amount suflicient to quickly precipitate said material without substantial attack upon the free fatty acid contained in said oil and immediately there after separating the preciptated gums from the oil.

44. The process as defined in claim 43, in which the oiland reagent, in stream flow, are quickly heated between the mixing and separation steps whereby to condition the mixture for separation.

45. The process of recovering crude lecithin from expressed vegetable oils which comprises the steps of pumping together predetermined measured ratios of the oil and an electrolyte constituting a coagulating agent and of a character and amount sumcient to efiect such coagulation without attack upon the free fatty acids or the oil, limiting the duration of the admixture to a brief period and promptly thereafter separating the precipitated material from the oil.

46. The processes defined in claim 45in which the electrolyte constitutes a preservative for the lecithin.

47. A continuous process for separating gums containing phosphatides and other impurities from fatty oils containing the same, comprising the steps of: admixing with said oils water as a precipitating reagent for said gums which will not substantially react with the free fatty acids contained therein and promptly and continuously, before injury to the oil by said reagent,

centrifugally separating the precipitated gums from the oil whereby to condition the same for subsequent refining for the removal of said free fatty acids.

48. As a product of manufacture, cottonseed phosphatides substantially free from linolenic acid and being predominantly acetone insoluble, the acetone insoluble portion of said phosphatides having a yellow color and containing about 2.6%

phosphorus.

' 49. As a product of manufacture, cottonseed oil phosphatides recovered from cottonseed oil,

said phosphatides being predominantly acetone insoluble, the dried acetone insoluble portion of said phosphatides being a yellow powder substantially free of linolenic acid.

50. As a product of manufacture, corn oil phosphatides recovered from corn oil, said phosphatides being predominantly acetone insoluble, the dried acetone insoluble portion of said phosphatides being substantially free from linolenic acid.

51. As a product of manufacture, vegetable phosphatidic material recovered from corn oil and characterized by being substantially free of linolenic acid.

52. As a product of manufacture, vegetable phosphatldic material recovered from cottonseed oil and characterized by being substantially free of linolenic acid.

BENJAMIN H. 'IHURMAN.

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