Agglomerated zeolitic adsorbents, method for obtaining same uses thereof
View Patent ↗The present invention relates to agglomerated zeolitic adsorbents based on zeolite X with an Si/Al ratio such that 1.15<Si/Al≦1.5, at least 90% of the exchangeable cationic sites of the zeolite X of which are occupied either by barium ions alone or by barium ions and potassium ions whose Dubinin volume is greater than or equal to 0.240 cm 3 /g. They are obtained by agglomerating zeolite powder with a binder, followed by the zeolitization of the binder, the exchange of the ions of the zeolite by barium ions (and potassium ions) and the activation of the adsorbents thus exchanged. These adsorbents are particularly suited to the adsorption of the para-xylene present in C 8 aromatic hydrocarbon fractions in the liquid phase in processes of simulated moving bed type but also to the separation of sugars, polyhydric alcohols, cresols or substituted toluene isomers.
1. Process for the recovery of para-xylene from C 8 aromatic isomer fractions in the liquid phase by adsorption of the para-xylene by an agglomerated zeolitic adsorbent in the presence of a desorbent the agglomerated zeolitic adsorbent comprising zeolite X and an inert binder, the inert binder containing at least 80% by weight of clay which has undergone zeolitization by the action of an alkaline solution, the zeolite X having an Si/Al ratio such that 1.15<Si/Al≦1.5 and having exchangeable cationic sites, wherein at least 90% of the exchangeable cationic sites of the zeolite X are occupied either by barium ions alone or by barium ions and potassium ions, the exchangeable sites occupied by potassium ions optionally representing up to ⅓ of the exchangeable sites occupied by barium ions and potassium ions, wherein the adsorbent has a Dubinin volume of greater than or equal to 0.240 cm 3 /g, the Dubinin volume being measured by nitrogen adsorption at 77° K after degassing under vacuum at 300° C. for 16 hours.
2. Process for the recovery of para-xylene according to claim 1 of simulated moving bed type.
3. Process for the recovery of para-xylene according to claim 2 of simulated countercurrent type.
4. Process for the recovery of para-xylene according to claim 2 of simulated cocurrent type.
5. Process for the recovery of para-xylene from C 8 aromatic isomer fractions in the gas phase by adsorption of the para-xylene by an agglomerated zeolitic adsorbent in the presence of a desorbent, the agglomerated zeolitic adsorbent comprising zeolite X and an inert binder, the inert binder containing at least 80% by weight of clay which has undergone zeolitization by the action of an alkaline solution, the zeolite X having an Si/Al ratio such that 1.15<Si/Al≦1.5 and having exchangeable cationic sites, wherein at least 90% of the exchangeable cationic sites of the zeolite X are occupied either by barium ions alone or by barium ions and potassium ions, the exchangeable sites occupied by potassium ions optionally representing up to ⅓ of the exchangeable sites occupied by barium ions and potassium ions, wherein the adsorbent has a Dubinin volume of greater than or equal to 0.240 cm 3 /g, the Dubinin volume being measured by nitrogen adsorption at 77° K after degassing under vacuum at 300° C. for 16 hours.
6. Process for the recovery of para-xylene according to claim 1 , wherein process the desorbent is toluene or para-diethylbenzene.
7. Process for the recovery of para-xylene according to claim 1 , wherein, in the binder present in the agglomerated zeolitic adsorbent used in said adsorption step, the clay is selected from the group consisting of kaolinite, halloysite, nacrite and dickite.
8. Process for the recovery of para-xylene according to claim 5 , wherein, in the binder present in the agglomerated zeolitic adsorbent used in said adsorption step the clay is selected from the group consisting of kaolinite, halloysite, nacrite and dickite.