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241.241.435/2571.435/259,435,306 07: 58 Field of Search USOO5951875A United States Patent (19) 11 Patent Number: 5,951,875 Kanel et al. (45) Date of Patent: *Sep. 14, 1999 54 ADSORPTIVE BUBBLE SEPARATION 5,332,100 7/1994 Jameson. METHODS AND SYSTEMS FOR 5,378,369 1/1995 Rose et al.. COMPONENTS THEREFROM 486999 2/1976 Australia. 487018 2/1976 Australia. 75 Inventors: Jeffrey Scott Kanel, Kingsport, Tenn.; O 523 883 1/1993 European Pat. Off.. Scott Arthur Guelcher, Weirton, Va. O 586 255 3/1994 European Pat. Off.. O 612 725 8/1994 European Pat. Off.. 73 Assignee: Eastman Chemical Company, 2367.705 5/1978 France Kingsport, Tenn 1541 345 2/1979 United Kingdom. s 20224.59 12/1979 United Kingdom. * Notice: This patent is Subject to a terminal dis- OTHER PUBLICATIONS CC. Rose, P.D. et al.; “Cross-flow Ultrafiltration Used in Algal 21 Appl. No.: 08/771,754 High Rate Oxidation Pond Treatment of Saline Organic 9 Effluents with the Recovery of Products of Value"; Water 22 Filed: Dec. 20, 1996 Science and Technology, 1992; Vol. 25, No. 10; pp. 319-327. 3.51 Int. Cl.C ................................210/703; AO1G 7.7100 BO1D2. 1/O2 Smith, P.H. et al., “Froth Flotation for Harvesting Chlorella O X O -- O "210/70,474. 241/. 241/2: 24/301; Algae'; Northwest Science, vol. 42, No. 4, 1968; pp. 241.241.435/2571.435/259,435,306 07: 58 Field of Search ................................. 210/703, 221.2, (List continued on next page.) 210/806, 768, 770; 47/1.4; 241/1, 2,301, 24.11; 435/259, 306.1, 283.1, 257.1 Primary Examiner Thomas M. Lithgow Attorney, Agent, or Firm-Bernard J. Graves; Harry J. 56) References Cited Gwinnell U.S. PATENT DOCUMENTS 57 ABSTRACT 3,268,606 8/1966 Jaeger. A proceSS and System are disclosed for recovering mixed 3,309,032 3/1967 Filz. carotenoids from the alga Dunaliella Salina. The harvested 3,479.281 11/1969 Kikindai. cells are ruptured, typically by circulating the algal Suspen E. 3.E. W. tal Sion at high pressure through a pump loop. The cells can 4,199.895 SE A.O. N. then be dewatered by absorptive bubble separation 4.253.271 3/1981 Raymond techniques, including a froth floatation circuit that has a 4341,038 7/1982 Bloch et al. roughing Zone and a concentrating Zone. If further concen 4,439,629 3/1984 Riegg. tration is desired, the algal concentrate can be mechanically 4,554.390 11/1985 Curtain et al.. filtered in a cross flow microfiltration unit in the absence of 4,680,314 7/1987 Nonomura. flocculating agents with Substantially no loSS of carotenoids 4,851,339 7/1989 Hills. in the permeate. Various methods for extracting mixed 4,938,865 7/1990 Jameson. carotenoids and other components from the algae are t so Not S. al. disclosed, including dense gas extraction, and extractions 516770s 12/1992 SN N. with natural and Synthetic flavorants, and edible oils. 5,188,726 2/1993 Jameson. 5,310,554 5/1994 Haigh. 36 Claims, 10 Drawing Sheets ET&I: SJSPE-3.- : : IM Miss Tika-LY FIR HE AL; SY 33.8%LY 8: II* IE x -SP 32 E R JRIFIai: OF s iCESS&3Y --- 5,951,875 Page 2 OTHER PUBLICATIONS L. J. Borowitzka et al., “Commercial Production of B-Caro Chemical Abstracts 85.400C; Vendt, V.P., “Experimental-in tene by Dunaliella Salina in Open Ponds’, Bulletin of dustrial Preparation of Carotene from Natural Brine Con Marine Science, 47(1), pp. 244-252 (1990). taining the Algae Dunaliella Salina'; Nov. 18, 1968; Vol. 69, I. Enes et al., “Optimization of Operating Strategies in No. 21, p. 7972. B-Caroteine Microalgae Bioreactors', Computers Chem. D.X. He., et al., “A Multiple-Loop Flotation Column For Enging, vol. 20 Suppl., p. S509 (1996). Wastewater Treatment”, Separations Technology 5 (1995), T.P. Moulton et al., “The Mass Culture of Dunaliella Salina pp. 133-138. for B-Carotene: From Pilot Plant to Production Plant”, N. Sammy, “Pilot B-Carotene Production: The Northern Hydrobiologia 151/152, pp. 99-105 (1987). Territory Experience”, Seventh Symposium On Salt vol. 1, G. Shele?, “High-Rate Algae Ponds For Wastewater Treat pp. 679–684 (1993). ment and Protein Production', Wat. Soi. Tech. vol. 14, pp. T.P. Moulton et al., “The Mass Culture of Dunaliella vividis (Volvocales, Chlorophyta) for Oxygenated Carotenoids: 439–452 (1982). Laboroatory and Pilot Plant Studies”, Hydrobiologia 204/ L. Schilpalius, “The Extensive Commercial Cultivation of 205, pp. 401–408 (1990). Dunaliella Salina”, Bioresource Technology 38 pp. 241-243 C.C. Curtain et al., “Manufacture of B-Caroteine from the (1991). Salt Lake Alga Dunaliella Salina; the Scientific and Tech S.S. Honeycutt, “A Technique for Harvesting Univellular nical Background, Australian Journal of Biotechnology, Algae Using Colloidal Gas Aphrons”, Biotechnology and vol. 1, No. 3, pp. 51-57 (1987). Bioengineering Symp. No. 13, pp. 567-575 (1983). U.S. Patent Sep. 14, 1999 Sheet 1 of 10 5,951,875 / STEP 2 O OBTAIN SUSPENSION OF OUNALELLA SALNA N BRINE FROM SOURCE 4. STEP 22 RUPTURE THE ALCAL BODES OPTIONALLY FILTER THE ALGAL BODES BY DEEP BED FLTRATION PERFORM ADSORPTIVE BUBBLE SEPARATIONS AS NECESSARY TO CONCENTRATE THE ALGAL SUSPENSION OPTIONALLY MICROFILTER THE ALGAL SUSPENSION EXTRACT THE CAROTENODS FROM THE CONCENTRATED AL.GAL SUSPENSON WITH SOLVENTS SELECTED FROM PETROCHEMICALS, FLAVORANTS, EDIBLE OLS, AND DENSE GASES –4. STEP 32 PERFORM SOLVENT EXCHANGE OR PURIFICATION OF COMPONENTS AS NECESSARY F.G. 1. U.S. Patent Sep. 14, 1999 Sheet 2 of 10 5,951,875 44- 36 64 F.G. 5 U.S. Patent Sep. 14, 1999 Sheet 3 of 10 5,951,875 1, 12 OO 1 OOO 8OO DAF TRATION STARTED 6 OO 4OO 2OO O 1 OO 2OO SOO 4OO TIME (MIN) A GAL FIG. 4. CONCENTRATE COLLECTION SEPARATION FEED ZONE ZONE 92 UNDERFLOW STREAM 82 BUBBLE GENERATION GAS ZONE FC 5. U.S. Patent Sep. 14, 1999 Sheet 4 of 10 5,951,875 -____~––).~--r ALGAL CONCENTRATE ––)------- UNDERFLOW FG 6. U.S. Patent Sep. 14, 1999 Sheet S of 10 5,951,875 FEED STREAM GAS 14O -144 - ALGAL ---------- N ----------, CONCENTRATE f STREAM FROTH FROTH ZONE ZONE 141 | | IN 154 IN-154 SEPARATION: :SEPARATION: ZONE ZONE N52 V12 f 136 138 -146 COLLECTIONZONE. - UNDERFLOW STREAM 154 U.S. Patent Sep. 14, 1999 Sheet 6 of 10 5,951,875 U.S. Patent Sep. 14, 1999 Sheet 7 of 10 5,951,875 198 ae 3 ea 2O6 196 19 O O th 194 1 N 182 -208 188 192 O Y. N 186 X 2O4 2O2 -DXH -DCH 184 -- : o 2-222 ALGAL UNDER FOW C-3 CONCENTRATE STREAM D{ G-3 GAS 185 FG 9. U.S. Patent Sep. 14, 1999 Sheet 8 of 10 5,951,875 WASH WATER FEED 212 UNDERFLOW 22O FC 1 O. U.S. Patent Sep. 14, 1999 Sheet 9 of 10 5,951,875 LNBOTHBEL 787 oxin-LEZ ENI?g—— U.S. Patent Sep. 14, 1999 Sheet 10 0f 10 5,951,875 5 OO CONTACT CONCENTRATED ALGAL SUSPENSION WITH SOLVENT –4 3O2 SEPARATE THE PHASES TO PRODUCE A CRUDE EXTRACT PHASE RICH IN CAROTENOIDS AND SOLVENT, A RAG LAYER OF AL.GAL RESIDUE, AND A RAFFINATE PHASE RICH IN BRINE 31 O /314 TREAT THE ALGA 512 M RESIDUE FOR CONCENTRATE EXCHANGE. F. RECOVERY OF CAR OTENOIDS NEEDED AND ERSE |N THE CRUDE RECOVER CHLOROPHYLSy EXTRACT SOLY AND OR OTHER COMPONENTS CAEPsU 516 PURFY MIXED CAROTENODS PRODUCT AS NEEDED F.G. 12 5,951,875 1 2 ADSORPTIVE BUBBLE SEPARATION Commercially, Dunaliella Salina normally is harvested METHODS AND SYSTEMS FOR from cultures that are produced in Specially constructed DEWATERING SUSPENSIONS OF outdoor ponds. The outdoor ponds typically are constructed MICROALGAE AND EXTRACTING in regions with a hot and arid climate with little rainfall and COMPONENTS THEREFROM few cloudy days to promote carotenoid production. Two distinct methods of aquaculture have been developed FIELD OF THE INVENTION for growing algae. These are an intensive mode and an extensive mode. Both aquacultural techniques require the The invention relates to methods for recovering compo addition of fertilizers to the medium to Supply the necessary nents from algae. More specifically, the invention relates to inorganic nutrients, phosphorous, nitrogen, iron, and trace methods for recovering mixed carotenoids from Dunaliella metals, that are necessary for biomass production through Salina. photosynthesis. BACKGROUND OF THE INVENTION The primary difference between the two modes of pro duction is mixing of the growth medium. Intensive ponds Carotenoids are deep yellow-orange pigments found in employ mechanical mixing devices while extensive ponds orange and yellow colored vegetables and in many dark 15 rely on mixing by the wind. Therefore, factors that affect green foods. Beta caroteine is the most abundant of the algae growth can be more accurately controlled in intensive various carotenoids. Beta caroteine can be converted by the aquaculture. body to vitamin A. Vitamin A is a fat soluble vitamin that can In both the intensive and extensive modes, the salinity of be stored in the body for a limited period of time, primarily the growth medium is controlled within a specified range, in the liver, unlike the water Soluble vitamins, which are not usually between about 18 to 27 percent sodium chloride by Storable. Vitamin Acan be toxic ifingested in large amounts. weight per unit Volume of brine. This range of concentra However, beta caroteine is converted by the body into tions is thought to provide the maximum carotenoid pro Vitamin A as needed and typically is considered a non-toxic duction. The optimum growth range for Dunaliella Salina is Source of Vitamin A even in large amounts.
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