Zeolite adsorbents comprising zeolite EMT, process for preparing the same and uses thereof

Patent metadata

Field	Value
Publication number	US-9707539-B2
Application number	US-201414888309-A
Country	US
Kind code	B2
Filing date	Apr 29, 2014
Priority date	Apr 30, 2013
Publication date	Jul 18, 2017
Grant date	Jul 18, 2017

Abstract

The present invention relates to zeolite adsorbents based on agglomerated crystals of zeolite EMT comprising barium and/or potassium. These adsorbents find applications in the separation of aromatic C8 isomer fractions, especially of xylenes, in the separation of substituted toluene isomers, such as nitrotoluene, diethyltoluene and toluenediamine, and in the separation of cresols, and in the separation of polyhydric alcohols, such as sugars.

First claim

The invention claimed is:

1. A zeolite adsorbent comprising zeolite EMT crystals and comprising barium and/or potassium, in which the total content of alkali metal or alkaline-earth metal ion oxides other than barium oxide BaO and potassium oxide K 2 O is between 0 and 5%, limits included, relative to the total mass of the adsorbent.

2. The zeolite adsorbent according to claim 1 , also comprising a non-zeolite phase.

3. The zeolite adsorbent according to claim 1 , wherein the zeolite EMT crystals have an Si/Al atomic ratio of between 1.00 and 2.00, limits included.

4. The zeolite adsorbent according to claim 1 , wherein the number-average diameter of the zeolite EMT crystals is between 5 nm and 1500 nm, limits included.

5. The zeolite adsorbent according to claim 1 , which also comprises crystals of at least one other zeolite, selected from the group consisting of zeolites of FAU structure, zeolites of LTA structure, and zeolites of MFI structure.

6. The zeolite adsorbent according to claim 5 , wherein the said at least one other zeolite is selected from the group consisting of zeolites of faujasite structure, alone or as a mixture and wherein the mass fraction of zeolite EMT is between 1% and 50%.

7. The zeolite adsorbent according to claim 1 , wherein the mass fraction of zeolite EMT is greater than 50% relative to the total weight of adsorbent.

8. The zeolite adsorbent according to claim 1 , comprising zeolite phases of EMT-FAU intergrowth.

9. The zeolite adsorbent according to claim 1 , wherein:
the barium content (expressed as a weight percentage of barium oxide BaO) is greater than 10% by weight relative to the total mass of the adsorbent, limits included,
the potassium content (expressed as a weight percentage of potassium oxide K 2 O) is between 0 and 25% by weight relative to the total mass of the adsorbent.

10. The zeolite adsorbent according to claim 1 , wherein the zeolite adsorbent has a loss on ignition, measured at 950° C. according to standard NF EN 196-2, of between 0 and 7.7% by weight.

11. The zeolite adsorbent according to claim 1 , wherein the zeolite adsorbent has a number-average diameter of between 0.2 mm and 2 mm, limits included.

12. A process for preparing a zeolite adsorbent according to claim 1 , comprising at least the steps of:
a) agglomerating a zeolite powder comprising zeolite EMT with a binder and forming, followed by drying and calcination, to obtain an agglomerate,
c) performing cationic exchange of the agglomerate by placing the agglomerate in contact with a solution of barium ions, or of potassium ions, or of barium ions and potassium ions,
d) optionally, exchanging with potassium,
e) followed by washing and drying of the product thus treated, and
f) activating the zeolite adsorbent thus obtained.

13. The process according to claim 12 , wherein step a) uses a binder containing at least 80% by weight of zeolitizable clay and a source of silica and the process comprises a step b) of zeolitization of the said binder by the action of an alkaline basic solution.

14. A zeolite adsorbent obtained according to the process of claim 12 .

15. A process using an adsorbent, wherein the adsorbent is a zeolite adsorbent in accordance with claim 1 and the process is selected from the group consisting of:
separation of aromatic C8 isomer fractions,
separation of substituted toluene isomers,
separation of cresols, and
separation of polyhydric alcohols.

16. The process according to claim 15 , wherein the process is the separation of para-xylene from aromatic isomer fractions containing 8 carbon atoms.

17. A process for recovering para-xylene from aromatic hydrocarbon isomer fractions containing 8 carbon atoms, in the liquid phase, by adsorption of para-xylene using a zeolite adsorbent in accordance with claim 1 in the presence of a desorbent.

18. The process for recovering para-xylene according to claim 17 , wherein the process is a simulated mobile bed process.

19. A process for recovering para-xylene from aromatic hydrocarbon isomer fractions containing 8 carbon atoms, in the gas phase, by adsorption of para-xylene using a zeolite adsorbent in accordance with claim 1 in the presence of a desorbent.

20. A process for separating polyhydric alcohols using an adsorbent, wherein the adsorbent is a zeolite adsorbent in accordance with claim 1 .

21. A process for separating substituted toluene isomers using an adsorbent, wherein the adsorbent is a zeolite adsorbent in accordance with claim 1 .

22. A process for separating cresols using an adsorbent, wherein the adsorbent is a zeolite adsorbent in accordance with claim 1 .

Assignees

• Ifp Energies Now
• Ceca Sa
• Arkema France

Inventors

• Bats Nicolas
• Laroche Catherine
• Leflaive Philibert
• Bouvier Ludivine

Classifications

• B01J20/3028

  Granulating, agglomerating or aggregating · CPC title

• B01J20/28007

  with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like (carbon nanostructures B01J20/205) · CPC title

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title

• C07C7/13

  by molecular-sieve technique · CPC title

• B01J20/186 Primary

  Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity · CPC title