Патент USA US2404037код для вставки
Patented July 16, 1946 0 2,404,037 UNITED STATES PATENT OFFICE 2,404,037 PROCESS or EXTRACTING BUTTER Loran 0. Buxton, Maplewood, N. J., assignor to National Oil Products Company, Harrison, N. J ., a corporation of New Jersey N 0 Drawing. _ Original application ~August 14, 1941, Serial No. 406,831. Divided and this an plication July 18, 1945, Serial No. 605,846 8 Claims. I This invention relates in general to the treat ment of butter and, more particularly, to im proved concentrated butter products and to cor~ related improvements in the process for produc ing the same. It is well known that the desirable delicate yet rich taste of many foods and food products, espe cially bakery products such as cakes, cookies, (01. 99-418) 2 effect on vitamin A must be employed. There fore, one must -be content with a poor yield of vitamin D or else risk destroying vitamin A. Fur thermore, a product produced by such a process has a tendency to be relatively unstable as a large part of the naturally occuring antioxidants in butter is left behind in the residue since a large portion thereof is nonvolatile under the tempera doughnuts and the like, is largely due to the use ture and pressure conditions which may be used of butter in the preparation of said products. In 10 and also, ‘by virtue of ' the high temperatures addition to imparting a very desirable taste and which are employed, some of the antioxidants flavor to food products by the use of butter, such which might be distilled are destroyed in the - use "will also enhance the nutrient value of the’ process. . foods since butter contains ‘certain vitamins, no It is the object of this invention to provide an tably A and D, whicZ . are essential to the health 15 emcient and simple process for the production of and well-being of humans. a product containing in their natural condition and in concentrated form substantially all the one could use a product which would have con ?avor-imparting and vitamin constituents and centrated therein all of the ?avor-imparting and natural antioxidants contained in butter. vitamin constituents of butter. Furthermore, at 20 Another object of this invention is to produce times it would be highly desirable to have all a product which will be liquid at ordinary ice box the ?avor-imparting and vitamin constituents of temperatures and which will contain in their a certain quantity of butter incorporated into natural condition and in concentrated form sub - an equal or smaller quantity of a product which stantially all the flavor-imparting and vitamin would remain liquid at ordinary ice box tem 25 constituents and natural antioxidants of butter. peratures. A further object of this invention is to produce In some cases it would be highly desirable if It has been proposed to prepare a butter con a butter concentrate which is stable towards oxi centrate by subjecting water-free butter fat to either short-path or molecular distillation. Such dative changes. Still another object of this invention is to pro a process has many disadvantages. Some of the 30 duce a butter concentrate containing relatively natural ?avoring constituents of butter have rela large quantities of vitamins A and D. tively high vapor pressures; in fact, some of these Other objects of the invention will in part be constituents are volatile at less than 100° C. when obvious and will in part appear hereinafter. under atmospheric pressure. In order to distill the vitamins in butter fat, the butter fat must The invention accordingly comprises the sev eral steps and the relation of one or more of such be heated to temperatures of around 200° C. un steps with respect to each of the others, and the der a high vacuum (0.1 mm. or less). Naturally, over such a wide range of conditions it will be composition possessing the features, properties and the relation of constituents, which are ex impossible to obtain clear-cut separation of the empli?ed in the following detailed disclosure, ‘and desired constituents but instead it can readily 40 the scope of the invention will be indicated in the be seen that if such a process is used there will claims. also be obtained in the distillate large quantities I have now discovered that if butter is con of high molecular weight glycerides which it is tacted with a suitable solvent which is substan desired to exclude. It has been admitted by the tially miscible with‘ the butter fat at room tem proposers of such processes that the product ob 45 perature or at temperatures substantially above room temperature and partially immiscible with tained by such a process is not all that is to be butter fat at temperatures substantially below desired as a certain amount of solids is not re room temperature, the solvent layer which sepa moved. To overcome this, successive distillations rates at the lower temperatures contains prac are usually carried out until the desired product is obtained. Naturally, such a process is very 50 tically all the ?avor-imparting and vitamin con costly and not practical commercially. stituents and natural antioxidants of the butter in their natural unchanged condition. This sol Another disadvantage of a molecular distilla vent layer may be removed from the immiscible tion process is that in order to obtain much of material and the solvent and miscible constit the vitamin D contained in the butter, a tempera ture which has a very harmful and deleterious 55 11611115 Separated by any Suitable means, 6- a. by 2,404,037 vacuum distillation, whereby a product contain ing a high concentration of vitamins, natural antioxidants and ?avor-imparting constituents prepared as hereinabove described may then, in accordance with the process of my invention, be is obtained. Substantially all the vitamin D as well as vitamin A present in the original butter are contained in the concentrate. Furthermore, the concentrate is highly resistant to oxidative changes since it has concentrated therein sub uct from the remainder of the oil. The tempera ture to which the solution is cooled may vary widely. In some cases it may be desirable to cool permitted to cool to effect a separation of the solution of the highly concentrated butter prod the solution to as low as —70° C. or lower. I have stantially all the natural antioxidants originally found, however, that proper layer formation is 10 obtained ii’ the mass is cooled to a temperature present in the butter. between about 10° and —20° C. Upon cooling. In carrying out the process of my invention the that part of the butter oil which will ordinarily solvent to be employed is selected from the class consisting of aliphatic esters containing 2 to 5 solidify may be removed from the solvent-oil mixture by ?ltration. This solid may again be carbon atoms. Usually the solvent should be one whose vapor pressure is not any less than that -15 extracted as hereinabove described and the ?nal residue which will thus be obtained is practically of any of the constituents of the butter as in re white in color, solid at room temperature and moving the solvent from the miscible portion of contains very little aroma or ?avor. This resi the butter fat, part of the ?avor-imparting con due is a pure fat which may be used as a shorten stituents may be lost. If desired or necessary, solvents of slightly lower vapor pressures may be 20 ing or in the production of margarine or for other similar purposes. used but the ?avoring quality of the product ob The combined solvent-oil extracts may then be tained will not be as good as in the case where treated in any usual manner to separate the a solvent of higher vapor pressure is employed. solvent from the 011, e. g., vacuum distillation, In any event the antioxidant and vitamin content s of the product will not be affected by the vapor 25 whereby an oil is obtained which is exceedingly more potent in carotene and vitamins A and D pressure of the solvent used. Solvents which I have found to possess the foregoing characteristics and properties are those falling within the class of aliphatic esters containing 2 to 5 carbon atoms. Solvents representative of this class are methyl formate, ethyl formate, ethyl acetate, beta-hy droxy ethyl acetate and vinyl acetate. Although it is preferred to remove most of the water from the butter before treating with the solvent, it is not absolutely necessary to do so. Occasionally it may be found that when most of the water has been removed from the butter, cer tain of the solvents mentioned hereinabove may be too miscible with the butter fat to produce by the process of my invention as highly a concen trated product as desired. However, this condi tion may be readily controlled by cooling to very low temperatures or by diluting the solvent with either a small amount of water or with some and contains most of the ?avors of the original butter. This oil also contains practically all the natural antioxidants which were originally pres ent in the butter. Thus the concentrated product produced by the process of my invention is far more stable than the original butter. Butter concentrates prepared as above de scribed are especially adapted for the ?avoring of foods, forti?cation of food products, cooking, carriers for vitamins, etc. These concentrates are liquid at ice box temperatures and may be used as such, or, if a liquid butter which is less concentrated is desired, the concentrates may be 40 added to some bland oil, such as corn oil, cotton seed oil, soybean oil, etc., which itself is liquid at ice box temperatures. Such a liquid product is excellent for use as a cooking oil and for similar purposes and is very stable against oxidative liquid organic solvent relatively immiscible with changes. mixture may then be heated until the oil or the imparting characteristics of butter. The product By arti?cially irradiating the milk from which butter fat. In general it may be said that the 45 the butter is made or irradiating the butter itself e?’ect of diluting any of the above solvents with with ultraviolet light to produce arti?cially ac water will be to render the solvents more im tivated vitamin D in the butter and then treating miscible with the butter fat, so that if diificulty is encountered in eifecting proper separation of the butter by the process of my invention, a con the desired products from the balance of the but 60 centrated product is obtained which is highly potent in vitamin D besides possessing all the ter fat, this di?iculty may generally be overcome by the addition of a small amount of water to other desirable characteristics herelnabove men tioned. the solvent. In carrying out the preferred process of my in If desired, the concentrated butter oil may be vention butter is ?rst melted by warming slowly, 55 added to lard or other nonbutter fats to produce shortening agents for the preparation of high thus allowing the whey (Water) portion to sepa quality bakery products. For some purposes rate from the butter oil. The butter oil is then butter is not as suitable a shortening agent as ?ltered while fluid in order to remove any traces some other types of oleaginous materials, e. g., of moisture. The relatively dry butter oil is then hydrogenated cottonseed oil. The product of my treated with the particular solvent to be em invention may be incorporated into hydrogen ployed. The relative proportion of oil to sol ated cottonseed oil or like shortening, thus pro vent may vary widely; preferably the ratio of ducing a product having the desirable character solvent to oil should be greater than one and in istics of a good shortening agent in addition most cases 4. to 50 parts of solvent to one part to the highly valuable nutritive and flavor 65 of butter oil is preferred. This solvent-butter oil of the invention may be used in lieu of drawn greater part thereof is dissolved in the solvent. (melted) butter which is usually served with I prefer to form the solution of oil in the solvent various seafood dishes such as lobster and by first heating the solvent to be used to a pre 70 steamed clams, and other dishes such as wa?es. determined temperature at which the oil when wheat cakes, etc. added will substantially completely dissolve in the The expression “butter” is used herein to con solvent and thenadding the oil to the solvent note ordinary butter, butter fat and butter oil. with agitation. This application is a division of my application The solution of the butter oil in the solvent Serial No. 406,831 ?led August 14, 1941. 5 2,404,037 Since certain changes in carrying out the above Process and certain modi?cations in the prod ucts which embody the invention may be made without departing from its scope. it is intended that all matter contained in the above descrip tion shall be interpreted as illustrative and not in a limiting sense. It is also to be understood that the following claims are intended to cover all the generic and 4. A process for producing a butter concen trate, the steps of which comprise contacting butter with vinyl acetate to dissolve a major por tion thereof, cooling the mass to a temperature below 10° C. to cause the formation of two layers and separating the vinyl acetate bearing in solu tion a major portion of the vitamin, ?avor-im parting and antioxidant constituents oi’ the butter. speci?c features of the invention herein de 10 5. A process for producing a butter concen scribed and all statements of the scope of the trate, the steps of which comprise dissolving at invention which as a matter of language might least the major portion of butter oil in a greater be said to fall therebetween. and that they are volume of a solvent selected from the group con intended to be inclusive in scope and not ex sisting of aliphatic esters containing 2 to 5 car clusive in that, if desired, other materials may bon atoms, cooling the mass to a temperature be be added to my novel composition of matter low 10° C. to cause layer formations and sepa herein claimed without departing from the spirit rating ‘the solvent layer having dissolved therein of the invention. Particularly it is to be under a major portion of the vitamin, ?avor-imparting stood that in said claims ingredients or compo and antioxidant constituents originally present nents recited in the singular are intended to in in the butter oil. clude compatible mixtures of said ingredients 6. A process for producing a butter concen wherever the sense permits. trate, the steps of which comprise dissolving at Having described my invention, what I claim least the major portion of butter oil in a greater as new and desire to secure by Letters Patent is: volume of ethyl formate, cooling the mass to a 1. A process for producing a butter concen 25 temperature below 10° C. to cause layer forma trate, the steps of which comprise contacting tions and separating the ethyl formate layer hav butter with a solvent selected from the group con ing dissolved therein a major portion of the vita sisting of aliphatic esters containing 2 to 5 carbon min, ?avor-imparting and antioxidant constitu atoms to dissolve at least a major portion of the ents originally present in the butter oil. butter, cooling the mass to a temperature at least 30 7. A process for producing a butter concen as low as 10° C. and separating from the mass the trate, the steps of which comprise dissolving at solvent bearing in solution a major portion of the vitamin, ?avor-imparting and antioxidant con stituents of the butter. least the major portion of butter oil in a. greater volume of ethyl acetate, cooling the mass to a temperature below 10° C. to cause layer forma 2. A process for producing a butter concen 35 tions and separating the ethyl formate layer trate, the steps of which comprise contacting but having dissolved therein a major portion of the ter with ethyl formate to dissolve a major portion vitamin, ?avor-imparting and antioxidant con thereof, cooling the mass to a temperature below stituents originally present in the butter oil. 10° C. to cause the formation of two layers and 8. A process for producing a butter concen separating the ethyl formate bearing in solution 40 trate, the steps of which comprise dissolving at a major portion of the vitamin, ?avor-imparting least the major portion of butter oil in a greater and antioxidant constituents of the butter. 3. A process for producing a butter concen trate, the steps of which comprise contacting but ter with ethyl acetate to dissolve a major portion thereof, cooling the mass to a temperature below 10° 0. to cause the formation of two layers and separating the ethyl acetate bearing in solution a major portion of the vitamin, ?avor-imparting 50 and antioxidant constituents of the butter. volume of vinyl acetate, cooling the mass to a temperature below 10° C. to cause layer forma tions and separating the vinyl acetate layer hav ing dissolved therein a major portion of the vita min, ?avor-imparting and antioxidant constitu ents originally present in the butter oil. LORAN O. BUXTON.