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4,466,923 34 Another object of the invention isto allow the use of pure CO2 for extraction without the need of entrainers forsolubilityenhancement. Other objects and advantages of the invention will become readily apparent from the ensuing description. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows the solubility of triglycerides in SC~ CO2 along various isotherms within the pressure range of 200-800 bar. FIG. 2 shows the solubility of triglycerides in SC CO2 along various isotherms within the pressure range of about 140-1240 bar. DETAILED DESCRIPTION OF THE INVENTION be explained in the following manner. Between its criti cal pressure of 74 bar and 400 bar, CO2 is quite com pressible. The density, which isrelated to solute holding power, changes rapidly in this range; whereas above 400 bar, the rate of change is less. Therefore, any in— crease in solubility with increase in temperature would be observed at the higher pressures; but at the lower pressures, the increased solubility effect due to tempera» ture may be overcome by the decrease in density and related decrease in solute capacity. The operating parameters .of the invention lie above the transition temperature and above 550 bar pressure. In the preferred mode, extractions are conducted in the temperature range of 60°—l00° C., and more particularly in the range 60°~80° C., and in the pressure range of 700—1200 bar. In actual practice, extraction efficiency is maximized at the highest temperature consistent with product integrity and at the highest practical pressure. Having selected one of the conditions, the other can be matched accordingly to give the optimum balance be tween solubility and energy input. The unexpected acceleration of isothermic solubility curves as a func The lipid-containing materials contemplated for de fatting by the method of the invention include any mate rial which exists in or which can be converted to a physical state that is permeable to the carbon dioxide under supercritical conditions, and in which the lipid therein is a fat or oil predominantly composed of a triglyceride.Exemplarymaterialsofplantandanimal25 tionofpressureabovethetransitionpoint,andthesensi origin without limitation thereto include: oilseeds, such as soy, cottonseed, sun?ower, safflower, peanut, and linseed; cereal components, such as corn germ; as well as animal byproducts, suet, offals, and the like. These materialsareconvertedtoanextractableformbycrush 30 theexamplesbelow,solubilitiesapproximating21% ing, grinding, comminuting, flaking, or other known method of making the oil physically available. were obtained with the normal solvent ?ow direction through the substrate from top to bottom. Substantially higher levels, however, would be predicted as attain able from the trend of the curves in FIG. 2. By revers ingthesolventdirectionto?ow frombottomtotopand applying relatively stringent conditions on the order of at least 70° C. and 800-850 bar, levels of extracted oil surpassing those indicated by the plots have been dem Any conventional supercritical ?uid extraction equipment comprising an extractor and separator would be suitable for carrying out the method of the invention. After packing the lipidcontaining material into the ex tractor, the SC-COZ is injected at the predetermined combination of temperature and pressure. Referring to FIG.1,itisapparentthatsolubilitiesoftriglyceridesat40 onstrated.Whileitistheorizedthatsomeoftheoil extraction temperatures of 55° C. or less follow the obtained by this latter method may not actually be dis predicteddensity-relatedsolubilitiestaughtbytheprior solved,therelativeweightofoiltoCO2yieldsapparent art. Likewise, the solubilities below about 400 bar relate inversely to temperature as previously observed. For instance, at 200 bar the solubility at 60° C. is only about 30% ofthatat50°C.,andat70°C.itisontheorderof 15% of the 50° level. The advantages of the invention become appreciable when temperatures ofatleastabout 60° C. and pressures exceeding 550 bar are simulta neouslyapplied.At 550barthesolubilityis23% greater at 60’ C. than at 50° C. and at higher temperatures and higher pressures, the differences are even more pro nounced. This effect is more clearly illustrated in FIG. 2. At 70'’ C. and approximately 825 bar, the triglyceride solubility in carbon dioxide is in excess of 20% by weight, as compared to about 2.8% at 40° C. and about 5% at55°C.atthesamepressure.Itisfurtherapparent from FIG. 2 that between 55° and 60° C., the solubility properties of SC-COZ undergo a dramatic transition. This phenomenon results in a decelerating rate of solu bility increase as a function of pressure below the transi tion temperature, and an accelerating rate above the temperature. While not desiring to be bound to any particular theory, the crossover effect between about 300 and 450 bar observed for isothermic solubility curves on either side of the transition temperature could solubilitiesupward of40%. The following examples are intended only to further illustrate the invention and are not intended to limit the scope of the invention which is de?ned by the claims. EXAMPLES l-48 A 4—l. vertically mounted and thermostated extrac tion cylinder having an 8.9-cm. inside diameter and safe operating pressure of 2000 bar at 25° C. was charged with ?aked triglyceride-containing substrate. The ex tractor was sealed and pressurized with CO2 injected from either the top or the bottom depending on the desired direction of flow. Dissolved oil was recovered in a separator by reducing the pressure to atmospheric. The percenttriglyceridesolubilitywas calculatedasthe ratio of the weight of collected oil to weight of CO2 solvent passed through the extractor times 100. The conditions and results of each run are reported in Tables I and II below. It is understood that the foregoing detailed descrip tion is given merely by way of illustration and that modi?cation and variations may be made therein with out departing from the spirit and scope of the invention. tivity of solute capacity to small changes in pressure, allows highly ef?cient recovery of dissolved oil in the separator by cycling pressure over a narrow range. At the endurance limit of the equipment employed inPDF Image | SUPERCRITICAL CO2 EXTRACTION OF LIPIDS
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