One-pot synthesis of copper containing small-pore zeolites

Patent metadata

Field	Value
Publication number	US-10486145-B2
Application number	US-201615765873-A
Country	US
Kind code	B2
Filing date	Oct 6, 2016
Priority date	Oct 12, 2015
Publication date	Nov 26, 2019
Grant date	Nov 26, 2019

Abstract

The present invention relates to a process for the manufacture of a copper containing small-pore zeolite which comprises⋅preparing a reaction mixture comprising a zeolite of the faujasite framework type, Cu-tetraethylenepentamine (Cu-TEPA) and at least one compound M(OH)x, which does not comprise the tetraethylammonium cation and⋅heating the reaction mixture to form a copper containing small-pore zeolite.

First claim

The invention claimed is:

1. A process for the manufacture of a copper containing small-pore zeolite which comprises
preparing a reaction mixture comprising a zeolite of the faujasite framework type, Cu-tetraethylenepentamine (Cu-TEPA) and at least one compound M(OH) x , wherein M is selected from the group consisting of lithium, sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, and barium, wherein x is 1 where M is lithium, sodium, potassium, rubidium, or cesium, and x is 2 where M is magnesium, calcium, strontium, or barium, and
in the absence of a tetraethylammonium cation, heating the reaction mixture to form the copper containing small-pore zeolite, and
wherein tetraethylenepentamine is the only organic molecule in the reaction mixture.

2. The process according to claim 1 , wherein the reaction mixture is an aqueous reaction mixture consisting of the zeolite of the faujasite framework type, the Cu-tetraethylenepentamine (Cu-TEPA), and the at least one compound M(OH) x .

3. The process according to claim 1 , wherein it is performed at temperatures of 80 to 150° C.

4. The process according to claim 1 , wherein it is performed at temperatures of 90 to 98° C.

5. The process according to claim 1 , wherein it is finished within 2 to 31 days.

6. The process according to claim 1 , wherein the zeolite of the faujasite framework type has a Si/Al ratio in the range from 2.4 to 30.

7. The process according to claim 1 , wherein the copper content of the copper containing small-pore zeolite is 1 to 10 wt %, calculated as CuO and based on the total weight of the copper containing small-pore zeolite.

8. The process according to claim 1 , wherein Cu-TEPA is used in an amount of 0.0001 mole/wt Cu-TEPA/FAU zeolite to 0.0016 mole/wt Cu-TEPA/FAU zeolite.

9. The process according to claim 1 , wherein the compound M(OH)x is CsOH and the copper containing small-pore zeolite obtained is of the ANA framework type.

10. The process according to claim 1 , wherein the compound M(OH) x is LiOH and the copper containing small-pore zeolite obtained is of the ABW framework type.

11. The process according to claim 1 , wherein the compound M(OH) x is NaOH and/or KOH and the copper containing small-pore zeolite obtained is of the CHA framework type.

12. The process according to claim 1 , wherein M(OH) x is used in an amount of 0.001 mole/wt MOH/FAU zeolite to 0.025 mole/wt MOH/FAU zeolite.

13. The process according to claim 1 , wherein seed crystals of the desired small pore zeolite are added to the reaction mixture.

Assignees

• Umicore Ag & Co Kg

Inventors

• Martens Johan Adriaan
• Sree Sreeprasanth Pulinthanathu
• Kerkhofs Stef Jules Peter
• Verheyen Elke Jane June
• Schuetze Frank-Walter

Classifications

• B01D2257/404

  Nitrogen oxides other than dinitrogen oxide · CPC title

• B01J2229/186

  not in framework positions · CPC title

• B01D2255/50

  Zeolites · CPC title

• B01J29/08

  of the faujasite type, e.g. type X or Y · CPC title

• B01J29/763 Primary

  CHA-type, e.g. Chabazite, LZ-218 · CPC title