Method for separating meta-xylene using a zeolitic adsorbent with a large external surface area

Patent metadata

Field	Value
Publication number	US-10125064-B2
Application number	US-201515501688-A
Country	US
Kind code	B2
Filing date	Aug 4, 2015
Priority date	Aug 5, 2014
Publication date	Nov 13, 2018
Grant date	Nov 13, 2018

Abstract

The invention relates to a method for separating meta-xylene from C8 aromatic fractions, using a zeolitic adsorbent based on sodium-exchanged or sodium-and-lithium-exchanged agglomerated crystals of zeolite Y, with a large external surface area.

First claim

The invention claimed is:

1. A process for separating meta-xylene from aromatic isomer fractions containing 8 carbon atoms, comprising contacting an aromatic isomer fraction containing 8 carbon atoms with a zeolite adsorbent comprising at least one faujasite-type zeolite Y comprising sodium or sodium and lithium, wherein
the zeolite adsorbent has an external surface area, measured by nitrogen adsorption, of greater than 40 m 2 ·g −1 , and wherein the external surface area is associated with a population of mesopores having a mean diameter of between 2 nm and 50 nm; and
meta-xylene is selectively adsorbed by the zeolite adsorbent.

2. The process of claim 1 , wherein the zeolite adsorbent has an external surface area, measured by nitrogen adsorption, of greater than 50 m 2 ·g −1 .

3. The process of claim 1 , wherein the zeolite a sorbent has an external surface area, measured by nitrogen adsorption, of 60 to 200 m 2 ·g −1 .

4. The process of claim 1 , wherein the zeolite adsorbent has a external surface area, measured by nitrogen adsorption, of 100 to 200 m 2 ·g −1 .

5. The process of claim 1 , wherein the zeolite adsorbent has an external surface area, measured by nitrogen adsorption, of 80 to 200 m 2 ·g −1 .

6. The process of claim 1 , wherein the zeolite adsorbent has a pore size, as determined via the Barrett-Joyner-Halenda method from the nitrogen adsorption isotherm at 77 K, for pores between 2 nm and 50 nm, that is unimodal and narrow.

7. The process of claim 1 , wherein the zeolite adsorbent is an adsorbent based on FAU-type zeolite(s) Y, wherein the zeolite adsorbent has a Si/Ai atom ratio of greater than 1.50.

8. The process of claim 1 , wherein the zeolite adsorbent has a mass fraction of FAU-type zeolite(s) Y of greater than or equal to 80% relative to the total weight of the zeolite adsorbent.

9. The process of claim 1 , wherein the zeolite adsorbent has a lithium content, of less than 8%, expressed as eight of lithium oxide Li 2 O relative to the total mass of the zeolite adsorbent.

10. The process of claim 1 , wherein the zeolite adsorbent simultaneously comprises pores having a diameter of greater than 50 nm, pores having a diameter of between 2 nm and 50 nm, limits not included, and pores having a diameter of less than 2 nm.

11. The process of claim 1 , wherein the zeolite adsorbent has macropores and micropores and wherein the zeolite adsorbent has a total volume contained in the macropores and the mesopores (sum of the macropore volume and of the mesopore volume) measured by mercury intrusion, of between 0.20 cm 3 ·g −1 and 0.70 cm 3 ·g −1 .

12. The process of claim 1 , wherein the zeolite adsorbent has a ratio (macropore volume)/(macropore volume+mesopore volume) of between 0.2 and 1.

13. The process of claim 1 , wherein the zeolite adsorbent has a micropore volume, evaluated by the t-plot method from the nitrogen (N 2 ) adsorption isotherm at a temperature of 77 K, of between 0.145 cm 3 ·g −1 and 0.350 cm 3 ·g −1 .

14. The process of claim 1 , wherein the zeolite adsorbent comprises mesoporous crystals of at least one zeolite Y, wherein the mesoporous crystals have a number-mean diameter of between 0.1 μm and 20 μm.

15. The process of claim 1 , wherein the zeolite adsorbent contains zeolite crystals and wherein the zeolite crystals are prepared by direct synthesis using one or more structuring agents or sacrificial templates.

16. The process of claim 1 , wherein the meta-xylene is separated by preparative adsorption liquid chromatography.

17. The process of claim 1 , wherein the zeolite adsorbent is an adsorbent based on FAU-type zeolite(s) Y, wherein the zeolite adsorbent has a Si/Al atomic ratio between 1.50 and 6.50.

18. The process of claim 1 , wherein the zeolite adsorbent has a lithium content of between 0 and 4%, expressed as weight of lithium oxide Li 2 O relative to the total mass of the zeolite adsorbent.

19. The process of claim 1 , wherein the zeolite adsorbent containing macropores and micropores and wherein the zeolite adsorbent has a total volume contained in the macropores and the mesopores (sum of the macropore volume and of the mesopore volume) measured by mercury intrusion, of between 0.20 cm 3 ·g −1 and 0.50 cm 3 ·g −1 .

20. The process of claim 1 , wherein the zeolite adsorbent has a ratio (macropore volume)/(macropore volume+mesopore volume) of between 0.4 and 0.8.

21. The process of claim 1 , wherein the zeolite adsorbent has a micropore volume, evaluated by the t-plot method from the nitrogen (N 2 ) adsorption isotherm at a temperature of 77 K, of between 0.205 cm 3 ·g −1 and 0.320 cm 3 ·g −1 .

22. The process of claim 1 , wherein the zeolite adsorbent comprises mesoporous crystals of at least one zeolite Y, wherein the crystals have a number-mean diameter of between 0.7 μm and 10 μm.

23. The process of claim 1 , which is conducted in a liquid phase or a gas phase.

24. The process of claim 1 , which is conducted in a counter-current adsorption unit.

25. The process of claim 24 , wherein the counter-current adsorption unit (a) has 6 to 30 beds, (b) has at least four operating zones, (c) is operated at a temperature between 100 C and 250 C, (d) a desorbent/feedstock flow rate ratio between 0.7 and 6.0, and (e) a recycling rate between 2.0 and 20.

26. The process of claim 1 , further comprising contacting the zeolite adsorbent with a desorption solvent.

Assignees

• Ifp Energies Now
• Ceca Sa
• Arkema France

Inventors

• Laroche Catherine
• Leflaive Philibert
• Baudot Arnaud
• Bouvier Ludivine
• Lutz Cecile
• Nicolas Serge

Classifications

• B01J20/28073

  being in the range 0.5-1.0 ml/g · CPC title

• B01J20/28059

  being less than 100 m2/g · CPC title

• B01J20/2803

  Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products · CPC title

• C07C15/08

  Xylenes · CPC title

• B01J20/28085

  being more than 50 nm, i.e. macropores · CPC title