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Latin American Applied Research 33:161-165 (2003) Carbon dioxide supercritical extraction provides low operating temperatures (that avoid product thermal deg- radation) and no solvent residue. The terpeneless oxy- genated aroma, of high commercial value, is obtained as the raffinate. Equilibrium predictions have been per- formed with the Group Contribution Equation of State (GC-EOS, Skjold-Jorgensen, 1984; Brignole et al., 1984). In this work, aldehyde pure group parameters have been calculated for GC-EOS, together with binary interaction parameters between this new group and par- affins, carbon dioxide and aromatics. Pure group and interaction parameters for olefin groups (Pusch and Schmelzer, 1993) and carbon dioxide and aromatics binary interaction groups (Bamberger et al., 1994) have been added to original GC-EOS parameters. Figure 2 shows binary phase equilibrium predictions for the sys- tem citral-carbon dioxide, with GC-EOS, which are in good agreement with experimental data (Marteau et al., 1995). 10 10 88 66 44 22 00 0.0 0.2 0.4 0.6 0.8 1.0 0.98 0.99 1.00 (x,y)CO yCO 22 Figure 2. Vapor-liquid equilibria for CO2 – Citral mix- ture The quality of ternary predictions has also been tested; Fig. 3 shows a pressure-composition diagram for a model lemon oil mixture (75% limonene and 25% citral), prepared by Kalra et al. (1987), with CO2, and our predictions at three isotherms. Figure 4 shows a comparison between GC-EOS va- por - liquid equilibrium predictions and the same ex- perimental data for the ternary. Finally, solubility data for an actual lemon oil-CO2 mixture (Kalra et al., 1987) have been compared to GC-EOS predictions for a 75% limonene-25% citral (weight) mixture in CO2, as it is shown in Fig. 5, at three different temperatures. Lemon peel oil can be accurately modeled as a binary mixture composed of limonene-citral (75-25 weight %) and pro- cess simulation and optimization have been performed for this lemon oil feed composition. Limonene 0.00 0.10 0.0 0.9 0.02 0.04 0.06 0.08 0.08 0.06 0.04 0.02 1.0 0.1 0.2 0.8 0.10 0.90 0.92 0.94 0.96 0.98 1.00 0.00 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Citral 0.0 354 K; 10.62 MPa 0.7 0.6 0.5 0.4 0.3 333 K; 10.32 MPa 0.2 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0.1 0.0 1.0 CO 2 Experimental data: Marteau et al., 1995 310 K 320 K GC-EOS predictions Experimental data (Kalra et al., 1987) 323 K 333 K 354 K GC-EOS calculations 16 14 12 10 8 6 4 2 0 Figure 4. Vapor-liquid ternary equilibrium diagram for CO2-Citral-Limonene mixture. (symbols: experimental data; lines: GC-EOS predictions) 6 4 2 0 0 2 4 6 8 10 12 14 16 Pressure (MPa) Figure 5. Predictions and experimental data for lemon oil solubility in CO2 III. OPTIMIZATION MODEL The determination of optimal solvent cycle scheme and operating conditions for the supercritical deterpenation of lemon oil has been formulated as the following 354.15 K 333.35 K 322.95 K Exp.data (Kalra et al., 1987) GC-EOS predictions CO +LMN/CITRAL(75/25 wt%) 2 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 CO2 weight fraction Figure 3. Pressure-composition diagram for the ternary mixture CO2-Limonene-Citral 162 Pressure (MPa) Pressure (MPa) Lemon oil solubility in CO2 (molar %)PDF Image | SOLVENT CYCLE DESIGN IN SUPERCRITICAL FLUID PROCESSES
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