2,412,707. Patented Dec. 17, 1946 UNITED STATES PATENT ornca Harold M. Barnett, Long Beach, Calif. No Drawing. Application June 7, 1943, Serial No. 489,990 8 Claims. This invention relates to the preparation of carotene in oil in concentrated form from vege table materials. ' (01. 260-666) , 2 remaining on the belt using a roller for this purpose. The amount of water to be used varies with different vegetables and with different lots having varying qualities and textures. I have The object of the invention is to provide a actually used up to 25 gallons of water to 100 process for recovering a concentrated solution of pounds of carrot pulp. The carotene in the carotene in oil from vegetable sources. Another water emulsion from this elutrlation or extrac object is to provide a process for making crystal tion process is then coagulated by heating the line carotene. liquid with or without a coagulant, or by means I have discovered that the carotene content of thoroughly pulped fresh vegetable such as car 10 of added coagulant such as hydrochloric‘ acid. When the carotene is to be subsequently trans rots may be almost completely removed by a formed from the water-base coagulum to an oil suitable water elutrlation process, and, when the solution, I prefer to add an inert ?lter-aid ma process is carried out with a minimum amount terial such as diatomaceous silica powder either of water, followed by subsequent coagulation of the carotene to form a water-dispersed coagulum 15 before or after the water-base coagulum is formed, or it ‘may be added at both stages. having as much as 50 to 200 or more times the The coagulum containing a small amount of original concentration in the carrots, the diatomaceous silica ?lter aid is separated from carotene may be obtained in oil solution by direct much of the water by decantation. The re extraction of the moist coagulum with hot vege table 011. 20 mainder of the liquid may be removed by ?ltra tion. Because of the slimy character of the My process will be illustrated by the prepara coagulum, even when ?lter-aid powder has been 6 tion of carotene from ‘carrots, although the proc added, the wet mass may be transferred to ?lter ess is applicable to other vegetable materials bags, allowed to drain, and then pressed to re having carotene content such as tomatoes, al move as much of the water as desired. The i’alia, sweet potatoes, etc. amount of ?lter-aid is chosen to produce a ?lter The fresh carrots are reduced to a pulp by able mixture without unnecessarily diluting the any suitable mechanical means, such as by pass carotene content of the cake. ing them through a hammer-mill preferably The moist coagulum containing?lter-aid as without added water or other liquid. It is im portant that the structure be well broken down 30 previously described, containing a high concen tration of carotene and a small amount of water, so that the carotene particles are released from may also be treated or extracted with a hot edible the ?ber and other materials. The semi-liquid oil such as cottonseed oil, to produce an oil solu mass or pulp is distributed in a thin layer on a tion of carotene. The temperature is main moving foraminous belt such as a screen belt, and jets of water are forced against the pulp on 35 tained at 100 to 150° C. Excess temperature and too long a time are to be avoided because of the the belt. The carotene and carotene-containing production of a scorched ?avor which is unde particles are insoluble in water, and are small sirable for uses in food. The oil is removed enough-some being of colloidal dimensions—to from the extracted dry solids by ?ltration or water. The action of the jets is to physically 40 centrifuging. If the residue contains much carotene, it may be again extracted with fresh disentangle the carotene particles from the ?ber oil, or the residue containing some carotene may and carry them through the screen, with avoid be used for the forti?cation of feeds. ance of formation of a mat of ?bers on the The carotene’ extraction from the moist ?lter ' screen which would act as a ?lter and hold back or entrap the carotene particles. I have found 45 cake is facilitated by forming the cake into rib bons or small rods (% to V4 inch in diameter) or that a screen of about 40 mesh is satisfactory pellets, by extrusion of the somewhat plastic mass for carrots, but the screen opening may be varied _ through a suitable die. By using counter-current for di?erent pulps. The minimum amount of extraction by the hot oil, I have been able to get water is used which will separate out substan tially all of the carotene particles. A moving 0 a high carotene concentration, for example, in belt has been found advantageous to keep the 5 one case as high as 1.5 percent carotene, equiva lent to 11,325,000 units of vitamin A per pound. amount of water to a minimum, but obviously When the oil solution of this concentration is other means may be used than those described cooled, as much as one-fourth of the carotene is here for illustration. When a belt is used, I ?nd be carried through the screen openings by the it desirable to press out the water from the pulp 55 deposited in crystal form, which can be separated 2,419,707 / ‘ 3 out by decanting or ?ltration, washed free from oil, thus recovering the carotene as a crystalline product... By avoiding the drying of the carrots in the initial step of the concentration, or of drying the concentrate, and using the method of extracting directly into the oil, I greatly decrease the cost 4 simultaneously dissolve out the carotene, and separating the oil from the solid residue. 4. The process of recovering carotene compris ing pulping a carotene-containing fresh vegeta ble. elutriating with water to separate the caro tene particles from the ?brous material, forming a moist solid coagulum containing the carotene, and extracting the carotene from the coagulum of getting the carotene from vegetable sources. The carotene oil concentrate is suitable for en richment of various foods and pharmaceuticals, 10 by means of hot edible oil. or it may be used directly as a source of vitamin ’ . mixture with edible oil to vaporize the water and ' 5. The process of recovering carotene compris ing pulping a carotene-containing fresh vegeta - ‘I claim: ble, elutriating with water to separate the caro 1. The process of extracting carotene from tene-containing particles from the ?brous mate solid moist fresh vegetable carotene concentrate 15 rial, adding a, ?lter-aid powder to the water sus comprising heating the concentrate with edible pension, forming a moist solidcoagulum contain oil to vaporize water and simultaneously extract ing the carotene and ?lter aid powder, forming the carotene in the oil, and removing the undis said coagulum ‘with ?lter-aid powder into small solved residue. , rods or pellets, and extracting said rods or pel 2. The process of recovering carotene compris» lets with hot edible oil to remove the carotene and 20 ing pulping a, carotene-containing fresh vegeta vaporize the water. ble, elutriating with water to separate the caro 6. ‘The process of claim 5, in which the extrac tene particles from the ?brous material, forming tion step consists. of moving said pellets or rods Y a solid coagulum of the carotene-containing par counter-currently against a stream 01' hot oil. ticles, separating the coagulum from excess wa 7. The process of making pure crystalline car 25 ter, heating the coagulum with edible oil to va otene comprising treating a moist solid carotene porize the water and simultaneously dissolve out concentrate with hot edible oil by counter-current the carotene, and separating the oil from the solid ?ow until said oil is, saturated with carotene, al lowing the oil solution to cool, and- collecting the 3. The process of recovering carotene compris separated crystals ofv carotene. , ' ing pulping a ‘carotene-containing fresh vegeta 30 8. The process of extracting carotene from a ble, elutriating with water to separate the caro moist fresh vegetable carotene concentrate com tene particles from the fibrous material, adding prising drying the concentrate to a solid, and ex. a ?lter-aid powder, forming a, solid- coagulum of tracting the solid concentrate with hot edible the carotene particles mixed with ?lter-aid, sep oil, l arating the coagulum and ?lter-aid from the ex 35 cess water, heating the coagulum and ?lter-aid residue. '