FROM BATCH ELUTION TO SIMULATED COUNTERCURRENT CHROMATOGRAPHY

Distillation is and will for quite a long time remain the main separation technique in the refining, petrochemical and chemical industries. Some separations however cannot be performed by distillation when the products to be separated are subject to thermal degradation or when their boiling points are too close. Under these circumstances adsorption or chromatographic processes are interesting alternatives. In the 1960's and in the early 1970's the technology of the simulated moving bed, the UOP rotary valve and the application of these devices to separation processes were introduced by UOP. Nowadays simulated "moving bed" or "countercurrent" separation processes may be found in the petrochemical industry where UOP still holds a quasi monopoly with the Molex process for n-isoparaffin separation and with the Parex process for paraxylene separation from C8 aromatic cuts. In the sugar industry competition is wide open. There are processes for glucose-fructose separation on the market (from Illinois Water Treatment, Mitsubishi Chemicals and UOP) while a xylose-arabinose-glucose separation and a sucrose extraction from molasses are available from Finn-sugar. Within this context Institut Francais du Petrole and Separex have developed the LICOSEP technology and propose its adaptation to different separations in the fine chemicals, pharmacy, perfumes and related industries. The principle of the simulated moving bed separation may be understood through the real countercurrent of a solvent and a solid selective adsorbing phase. In the mixture to be separated some of the components are relatively adsorbed while the other ones are not. The operations consist in adjusting the different flowrates so that the adsorbed compounds will be entrained with the solid while the nonadsorbed compounds will travel along with the liquid solvent. Actually the circulation of a solid phase is technically difficult. This operation is simulated by permutations of injected and withdrawn streams through multiple ports located all along the separation column. The practical construction of three pilot plants working according to the simulated moving bed technique is shown. Twenty-four columns filled with a fixed phase are mounted in series. A metering pump is fitted between the 24th and the first column in order to create a recirculation stream. Between each two columns it is possible to inject the feed or the solvent stream or to withdraw either the extract or the raffinate stream. These four streams flow continuously and each of them is directed by a twenty-four position valve to the right intercolumn assembly depending on the period of the cycle. Solvent injection, feed injection and extract withdrawal are performed by metering pumps while the raffinate withdrawal is done by an upstream pressure-control valve. The four multiposition valves, the four metering pumps, the pressure control valve and various side devices such as online analyzers of the effluents are commanded by a computer. Two examples of separation performed in these pilot plants are shown: paraxylene separation from C8 aromatic feedstock and xylose separation from xylose-arabinose-glucose mixtures. The experiments performed made it possible to determine both static and dynamic parameters of the process. The main conclusion is that a modelization of the plant is necessary not only for process optimization but also to correctly operate these units. We have developed a model that accurately represents the separation of binary mixtures. Generally multicomponent separations are more difficult to represent and in this respect our model predictions are only qualitative ones. A guideline is then given for making choice between conventional elution chromatography and simulated moving bed separation. Some improvements in this process are also discussed. A five-zone simulated moving bed with reinjection of distilled extract provides great increases in extract purity. It is also possible to combine preparative supercritical chromatography with a simulated moving bed in a six-zone scheme in order to continuously separate three effluent streams. Thus great extensions of the field of application of simulated moving bed separations are expected in the coming years.