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1. Field of the Invention 4,466,923 12 bar, and 50° C. at 350 bar. The paper also states that the solubility of a substance in a supercritical gas depends primarily on the density of the gas. Likewise, Johnston etal.[AIChEJournal27(5);773-779(September1981)] 5 concludesthatsolubilitycorrelatesbestwithdensityas an independent variable and isin fact linear on a plot of Essentiallyaloftheoilfromthemorethan30million logsolubilityvs.solventdensity.Accordingto‘Hubert tons of soybeans as well as millions of tons of other et al. (“Extraction with Supercritical Gases,” G. M. oilseedsandgraincommoditiescrushedannuallyfor Schneider,E.Stahl,&G.Wilke,eds.,VerlagChemie, SUPERCRITICAL CO2 EXTRACTION OF LIPIDS FROM LIPID-CONTAINING MATERIALS BACKGROUND OF THE INVENTION use in the United States is extracted with hexane. Prob lems associated with the use of this solvent are numer ous. It is highly flammable and explosive when mixed with air. It is also not selective for triglycerides result ingintheconcurrentextractionofundesirableimpuri tiesincludingfreefatyacids,phospholipids,pigments,15 C.takeplacefrom'70to150barandthatbothparame and unsaponi?ables. Signi?cant re?ning losses and at o Deer?eld Beach, FL, 1980, pp. 27-28) extraction with supercriticalCO2 offerstheadvantagesofbeingableto varythedensityand‘dielectricconstantsbyvaryingthe pressure. This reference shows’ graphically that the tendant energy requirements to remove such impurities contributetoproductioncosts.Moreover,withthe 3‘pectedbyemployingCO;atpressuresmuch'inexcessof rapidlyescalatingcosts,uncertainavailability,andpo tentialhealthandsafety-relatedproblemsofhydrocar 20 bon solvents in general, the social and economic envi ronment has stirred interest in alternatives. 300 bar would not justify the additional energy re quired. Furthermore, Stahl et al. (Fette '...,supra), teaches in Table I that increasing temperature at con stant pressure reduces the solubility of triglyceride in CO2. In accord with that observation, the preponder Supercritical ?uids technology may be a viable alter native to current extraction methods. Supercritical ?u ids(SCF’s)areoftenreferredtoasdensegases.Techni 25 anceoftheartconcursthatforoilsandotherlowvola cally,anSCF isagasexistingaboveitscriticaltempera ture and critical pressure, as de?ned in the phase dia gramofthepuresubstance.When agasiscompressed aboveitscriticaltemperature,densitiesincreasedramat ically. Therefore, under a given set of conditions, an SCF may possessthedensityofaliquidwhilemaintain ing the diffusivity of a gas. The solvent properties of SCF’s have been recognized for over 100 years but commercial applications have been slow in developing. As far as isknown, decaffeination of coffee with super critical carbon dioxide (SC-CO2) is the only current large-scale commercial SCF process. SC-COZ is an ideal solvent because it is nontoxic, nonexplosive, cheap, readily available, and easily re movedfromtheextractedproducts.Moreover,prelimi 40 naryunpublishedresultsofFriedrichetal.indicatethat the levels of pigments, iron, and phosphorus extracted from soybeans by SC-CO; are signi?cantly less than those extracted by hexane. 2. Description of the Prior Art ' SC-COZ has been investigated as an extracting sol vent in the processing of a vast array of oleaginous products.One ofthe?rstteachingsofthissortisfound inBritishPat.No. 1,356,749‘whereinavarietyofvege table oils were separated with SC-COZ from their re spective seeds. Similar applications include the extrac tion of fats and oils from cocoa solids (British Pat. No. tility substances the solubility in SC-COZ is maximized at temperatures slightly above the critical point. The 3% byweightsolubilityofsun?owerseedoilreported by Stahl et al. [J. Agr. Food Chem. 28(6): 1153-1157 (1980)] at 40° C. and 700 bar is typical of the results obtainedbypriorartprocesses.Inlightoftheseobser vations, prior disclosures of extreme conditions (up to 2000 excess atmospheres and 170° C., U.S. Pat. No. 3,843,824) have been no more than academic curiosities. With a plurality of polar compounds, Stahl etal. [Ag new. Chem. Int. Ed. Engl. 17: 731-738 (1978)] shows in FIG. 11 a decelerating rate of solubility increase as a function of pressure up to about 2500 bar at 40° C. SUMMARY OF THE INVENTION I.have now surprisingly discovered that when SC CO; is used to extract a lipid‘from a lipid-containing substance at a temperature in excess of about 60° C. in combination with a pressure in excess of 550 bar, the solubilityofthelipidintheCO2solventisdramatically increased over levels heretofore observed. Moreover, I’ have unexpectedlydiscovered that the solubility in creases at an accelerated rate as the pressure increases along any given isotherm above about 60° C. These responses are in direct contrast to all the previously discussed teachings in the art, in which solubility has been shown to be an inverse function of temperature, and in which accelerated rates thereof have been attrib uted only to lower pressures in the range of about 1,356,750), starch-containing vegetable materials (Schwengers, U.S. Pat. No. 3,939,281), chamomile (Stahletal.,GermanPat.No.2,709,033),animalprod 55 70-400bar. ucts (U.S. Pat. No. 4,280,961), and lupine seeds [Stahl et In'accordance with this discovery, it is an object of al.,Fette,Seifen,Anstrichmittel83(12):472-474 theinventiontoprovideanefficientandeconomical (1981)].Additionally,Caragayleta1.[presentationatthe 72nd Annual Meeting of American Oil Chemists Soci ety,NewOrleans,LA(May18,1981)]urgesthatSC 60lipidsbymeansof‘aSC-COZsolvent. COz can be used to effectively fractionate and purify heat-abused oxidized cooking oils. In a review paper by Brunner et al. entitled “The State of the Art of Extraction with Compressed Gases” (lecturepresentedatAnnualMeetingofProcessEngi 65 neers, Strassburg, Oct. l-3, 1980), typical temperature and pressure parameters for extraction of seeds oils with supercriticalCO;were 130°C.at150bar,40'C.at220 It is also an object of the invention to signi?cantly reducethetime,energy,andCog-consumptionrequire ments for lipid extraction under, supercritical condi tions. It is a further object of the invention to enhance the solubilityoffatsandoilsincarbondioxidebyafactorof up to four or more over that previously taught in the priorart. greatest change in density and dielectric constant at 50° ters increase only slightly above about 300 bar. It is clear therefrom that the increased solubility to be ex method for both the‘extraction and fractionation ofPDF Image | SUPERCRITICAL CO2 EXTRACTION OF LIPIDS
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