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Solvent Cycle, Methods for Solute Precipitation Heat and Mass Transfer: High Pressure chemical Engineering I (WS) Chapter 7
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Flow Scheme of a Solvent Cycle
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Solvent Cycle Steps: separate the extract from the solvent (1), clean the solvent for reuse (2), remove the solvent from raffinate (3), adjust composition of solvent mixture (if applicable) (4). Solvent Cycle
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Single stage Multiple stage Counter- Chromato- (precipitation) current graphic SFE Modes of Operation
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Extraction From Solids S t S / F Essential oils(5 %) 20 20 Edible oils(2 %) 40 < 1 40 Coffee decaffeination (0.01 %) 200 5 40 Black tea decaff. (0.01 %) 230 1.5 150 Total amount of solvent S, kg/kg F Extraction time t, h Solvent to Feed Ratio S/F, kg S /(kg F h) Basis: Solvent: Carbon dioxide 10 - 30 MPa, 330 K Solvent Cycle: Solvent to feed ratio of SFE processes
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Countercurrent Separation V/L v S / F FAEE, FAME (5 %) 20 7.5 125 FFA (fatty acids) (2 %) 50 4.5 50 Squalene (1.5 %) 20 10 50 Tocopherol-Purif. (2.5 %) 35 20 45 Solvent ratio V/L, kg/kg Reflux ratio v, - Solvent to feed ratio S/F, kg F /kg F Basis: Solvent: Carbon dioxide 10 - 30 MPa, 350 K Solvent Cycle: Solvent to feed ratio of SFE processes
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Chromatographic Separation P r t r S / F DHA / DPA 1.5 15 900 x 10 3 EM Phytol-isomers 10- 30 6 900 EM 200 SMB Productivity Pr, g P /(kg StPh h) Retention time, min Solvent to feed ratio S/F, kg F /kg F Basis: Solvent: Carbon dioxide 10 - 30 MPa, 310 K Solvent Cycle: Solvent to feed ratio of SFE processes
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Reduction of pressure or density Anti solvent Membrane separation Adsorption Absorption De-Entrainment...... Modes For Product Recovery
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Birtigh, Brunner, Johannsen Solubility of Caffeine in CO 2
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Gas Circuit in the Compressor Mode
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Compressor Process, Throttling Sub-Critical
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Compressor Process, Throttling Super- Critical
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Pump Process
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Pump Process, Throttling, Sub-Critical
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Pump Process, Throttling Super- Critical
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Extraction temperature: 313 K Energy Consumption by Various Solvent Cycles
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Mechanical Energy Thermal energy in Thermal energy out Pump with heat recovery Pump without heat recovery Compressor with heat recovery Compressor without heat recovery Extraction pressure [MPa] Energy [kJ/kg] Energy needed for the gas cycle 70 kJ/kg CO2 95 kJ/kg CO2 for S/F 125 kg/kg: 8750 kJ/kg Feed 11875 kJ/kg Feed
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Reduction of pressure or density (temperature) Anti solvent Membrane separation Adsorption Absorption De-Entrainment Modes For Product Recovery
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Brunner 1983 Solubility in a Gas With a Modifier (Entrainer) Influence of temperature
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Data by: Gährs 1984 Ebeling, Franck 1984 Johannsen, Brunner 1994 Solubility of Caffeine in CO 2
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Reduction of pressure or density Anti solvent Membrane separation Adsorption Absorption De-Entrainment...... Modes For Product Recovery
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Gährs 1984 Anti-Solvent: Solubility of Caffeine in CO 2 Influence of nitrogen
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Reduction of pressure or density Anti solvent Membrane separation Adsorption Absorption De-Entrainment...... Modes For Product Recovery
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Solvent Cycle With Membrane Separation
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GKSS-membrane (organic, active dense layer) CO 2 OC Permeate Retentate 1.86 wt.-% < 0.06 wt.-% p = 2.0 MPa active dense layer 1.5 mole CO 2 kg/(m 2 h) P = 18 MPa, T = 323 K Separation by Membranes
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Solvent Cycle in a T,s - Diagram Extraction/ separation Precipitationat high p Precipitation at low p Compressormode Entropy Temperature CO 2
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53 kJ/ kg CO2 21 kJ/ kg CO2 7.6 kJ/ kg CO2 Like in 2 Energy For Different Solvent Cycles Pump-Cycle Compressor-Cycle Membrane-Cycle Sartorelli 2001
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Reduction of pressure or density Anti solvent Membrane separation Adsorption Absorption De-Entrainment...... Modes For Product Recovery
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Adsorption of Caffeine on Activated Carbon
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Silica with 52% loading, loaded by high pressure adsorption Silica with 50% loading, loaded by mixing, conventional process Recovery of Tocopherolacetate by Adsorption
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Reduction of pressure or density Anti solvent Membrane separation Adsorption Absorption De-Entrainment...... Modes For Product Recovery
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Phase Equilibrium Caffeine - Water - CO 2
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Reduction of pressure or density Anti solvent Membrane separation Adsorption Absorption De-Entrainment...... Modes For Product Recovery
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Brunner 1983 Solubility in a Gas With a Modifier (Entrainer) Influence of temperature
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Birtigh De-Entrainment
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Generalization of Precipitation: Membership - Functions Temperature at the Swimming Pool T [ o C] x 253545 0 1 (x) (x) „Hot“ Not yet hot Too hot (x): relative number of statements from people at the pool
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Birtigh Membership Functions P Adsorption Membrane
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Absorption De-Entrain T T Birtigh Membership Functions
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