Supercritical fluid extraction on semibatch mode for the removal of terpene in citrus oil

Supercritical carbon dioxide extraction of a mixture of limonene and linalool was carried out with a rectification column in the semibatch operation mode. For the simple semibatch extraction where the column was controlled at the uniform temperature without an internal reflux, the Rayleigh equation, developed for the simple batch distillation, was applied to express the dynamic extraction behavior. In this paper the Peng−Robinson equation of state was used to estimate the ternary phase equilibria. The semibatch extraction with internal reflux induced by a temperature gradient of the rectification column increased the separation selectivity. The internal reflux ratio was calculated by the measurement of the extraction rates at the top and bottom of the column, and it was 7.6 for the column having a temperature gradient from 313 K at the bottom to 333 K at the top at 8.8 MPa. Behavior in the rectification column was discussed by means of estimated physical properties.