US2103193A - Process for the recovery of the unsaponifiable fractions of oils - Google Patents

Description

Patented Dec. 21, 1937 1 PROCESS FOR THE RECOVERY OF THE UN- SAPONIFIABLE FRACTIONS OF OILS Robert Preston Nichols, Miami, Fla., assignor to Edward L. Nichols, Hollywood, Fla.

No Drawing. Application September 19, 1933, Serial No. 690,107

2 Claims. (Cl. 260-153) My invention relates to a process of recovering the contents into the pans as soon as the mass unsaponifiable fractions of fats, and is particubecomes thick. Ordinarily a cool solidified soap larly adaptable for use in extracting suchfracmass will be formed in not over twenty minutes tions of cod liver oil, shark liver oil, and the like. from the time the lye is added to the container.

The invention, which has among its objects a The soap mass formed as above described conquickly performed process requiring inexpensive tains mixed with it the unsaponifiable portions apparatus, will be best understood from the folcontaining the vitamins A and D. The soap mass lowing description of several examples of the may now be treated to remove these portions. practice of the process, while the scope of the Preferably this is done by first breaking up the m invention will be more particularly pointed out in soap mass, and then treating it with a volatile the appended claims. organic solvent for the unsaponifiable matter.

As is well known, the unsaponifiable portions As suitable solvents, ether, carbon tetrachlorid, of fats, such as cod liver and shark liver oils, chloroform, or the like, in which the soap and contain the valuable vitamins A and D. As the alkali are only minutely soluble, may be em- ]5 improved process lends itself to performance with ployed. Conveniently, the pans employed for a minimum of exposure of the materials to air, solidifying the soap mass may be in the form of light and moisture, it is particularly adaptable troughs to cause the solidified mass to be in the for extracting these vitamins, the latter, particuform of elongated sticks say, for example, sticks larly vitamin A, being susceptible to destruction about one inch square, these being readily pre- 90 when the material is so exposed. sented to a grinding machine which will break As one manner of practising the present invenp h S p into a o se Pow ertion, but without limitation thereto, the fatty ma- The xtr t n f the n pon fi le p rtions terial, such as cod liver oil, may be placed in a from the P d d broken 1 Seal) mass y container, after .which is added dry powdered be p r rm d y p a th s ap p wd r n a sodium hydroxid in the form of co me i l l container and adding the ether orother volatile for example, one containing about 98% sodium S vent a d Stirring e nt ts f e Conhydroxid. the lye being added preferably as a tainer. Upon being allowed to stand the soap mass as distinguished from gradually adding it, will settle at the bottom of the container, after Preferably, the amount of lye added is such as Which the liquid Contents may be decanted,

to present an amount of sodium hydroxid in expri r t s ttl n the s ap may be s pa ated fr m 30 cess of that necessary to saponify the saponifiable the qu d by us f a tr u al s parat r r y fats in the oil, so as to cause the moisture to be use Of a filter- It has b found that ug y 10 absorbed and the vitamins to be thus protected p s v nt to one p rt ap will i i fa from this moisture. In practice, equal portions Y results, but these P op are y I10 by weight of the oil and sodium hydroxid in the fii C t calform of commercial lye give satisfactory results. The ether or other solution of the unsaponi- Immediately upon introducing the lye the confiable fractions, separated as above described,

tents of the container are intimately mixed as, for may be then treated by a distilling operation to example, by use of a mechanical mixer. Pracremove the solvent, distillation preferably being tically immediately, saponification begins, the performed under reduced pressure and at a 40 temperature of the contents of the container rlstemperature not exceeding 100 C. By this means ing rapidly and saponification proceeding at a a concentrate rich in the vitamins A and D is rapid rate, so that in a few minutes the mass recovered. Any small fraction of soap present becomes thick and pasty. At this point the main the concentrate may be removed, if desired,

terial is preferably poured into pans to permit the by treating the concentrate with a small amount 45 saponification reaction to become complete and of ether, or other of the above mentioned solthe material to cool and harden into a block of vents in which the soap is only very slightly solusoap, If desired, the oil may be slightly heated ble, to dissolve off the unsaponifiable matter and before adding the lye to initiate the saponificaleave the soap behind, or the concentrate, which tion reaction, but ordinarily this will be unordinarily is in the form of a rather thick paste, 50 necessary. Preferably, care should be taken not may be diluted with cod liver oil, corn oil, cotton to give such an initial heating as will cause the seed oil, peanut oil, or the like, in which the soap temperature of the mass, when the reaction 00- is not soluble, and the solution filtered or subcurs, to rise above from to C. This ex- ,iected to centrifugal action to remove the soap.

55 cess temperature may be prevented by pouring Commonly the concentrate is used to enrich the 55 vitamin content of cod liver or other oils, and may be added thereto, and any soap present may be removed by filtering or centrifugal action.

In the above examples of the practice of the invention, any residual amount of ether or other solvent present in the separated soap may be recovered for reuse, preferably by a distilling operation.

It will be observed in the above examples of the practice of my improved process, that the excess of lye or other hydroxid added to the oil not only saponifies the fatty fractions, but being in amount in excess of that necessary to form the soap, also takes up the moisture so that the unsaponifiable fractions are not subjected to moisture during the process. This materially aids in the recovery of a high percentage of the vitamin A which tends to be destroyed, at least in part, when subjected to moisture, particularly in the presence of heat.

It will be understood that wide deviations may be made from the above examples of the practice of my invention without departing from the spirit thereof.

I claim:

1. The process of recovering the unsaponifiable fractions of fish liver oil which comprises adding to and immediately mixing with the oil dry powdered sodium hydroxide, the latter being added to the oil substantially as a mass in large excess over that necessary to saponify the saponifiable fractions of the oil, so as to absorb moisture for protecting the vitamins and cause to be quickly formed a solidified mixture of soap and sodium hydroxide of requisite hardness to be reduced to a powder by a grinding operation; operating upon said solidified mixture to grind it to a powder; treating the resulting powder with ether for dissolving the unsaponified fractions of the oil; separating the powder from the ether solution; and distilling the ether from the powder free ether solution to obtain a concentration of the unsaponifiable fractions of the oil.

2. The process of recovering the unsaponifiable fractions of fish liver oil which comprises adding to and immediately mixing with the oil dry powdered sodium hydroxide, the latter being added to the oil substantially as a mass in large excess over that necessary to saponify the saponifiable fractions of the oil, so as to absorb moisture for protecting the vitamins and cause to be quickly formed a solidified mixture of soap and sodium hydroxide of requisite hardness to be reduced to a powder by a grinding operation; operating upon said solidified mixture to grind it to a powder; treating the resulting powder with a volatile liquid in which both the unsaponifiable and saponifiable fractions of the oil are soluble, but in which both the soap and sodium hydroxide are insoluble, for dissolving the unsaponified fractions of the oil from the powder; separating the powder from the resulting solution of the unsaponified fractions of the oil; and treating the powder free solution for vaporizing the volatile liquid solvent therefrom to obtain a concentration of the unsaponifiable fractions of the oil.

ROBERT PRESTON NICHOLS.