AEI zeolite synthesis

Patent metadata

Field	Value
Publication number	US-9919296-B2
Application number	US-201414529647-A
Country	US
Kind code	B2
Filing date	Oct 31, 2014
Priority date	Oct 31, 2013
Publication date	Mar 20, 2018
Grant date	Mar 20, 2018

Abstract

A novel method for synthesizing AEI zeolites is provided which results in high overall relative yields on silica and the structure directing agent. Structure directing agents useful in the present invention include the cations N,N-Dimethyl-3,5-dimethylpiperidinium, N,N-Dimethyl-2-(2-hydroxyethyl)piperidinium, N,N-Dimethyl-2-ethylpiperidinium, and 2,2,4,6,6-Pentamethyl-2-azoniabycyclo[3.2.1]octane.

First claim

What is claimed is:

1. A zeolite synthesis method comprising:
forming an AEI zeolite reaction admixture comprising a mother liquor, or portion thereof, from an AEI synthesis process, wherein the mother liquor, or portion thereof, comprises an AEI structure directing agent; a source of silica, a source of alumina, and a source of hydroxide ions, and
reacting the admixture under crystallization conditions to form a batch of zeolite crystals having an AEI framework and a subsequent mother liquor;

wherein the structure directing agent is one or more cations selected from N,N-Dimethyl-3,5-dimethylpiperidinium, N,N-Dimethyl-2-(2-hydroxyethyl)piperidinium, N,N-Dimethyl-2-ethylpiperidinium, and 2,2,4,6,6-Pentamethyl-2-azoniabycyclo[3.2.1]octane.

2. The zeolite synthesis method of claim 1 further comprising:
separating the zeolite crystals having an AEI framework from the subsequent mother liquor; and
using the subsequent mother liquor, or a portion thereof, to synthesize one or more sequential batches of zeolite crystals having an AEI framework.

3. The zeolite synthesis method of claim 2 , wherein the subsequent mother liquor, or a portion thereof, is used to synthesize X sequential batches of zeolite crystals having an AEI framework, and wherein X is an integer having a value effective to produce an overall relative yield on silica of at least about 60 percent and/or an overall relative yield on structure directing agent of at least about 40 percent.

4. The zeolite synthesis method of claim 3 , wherein X is 1 to 20.

5. The zeolite synthesis method of claim 1 , wherein the structure directing agent is N,N-Dimethyl-3,5-dimethylpiperidinium cation.

6. The zeolite synthesis method of claim 1 , wherein the use of the mother liquor, or a portion thereof, in a series of sequential AEI zeolite synthesis batch reactions results in an overall relative yield on silica of at least about 60 percent and/or an overall relative yield on structure directing agent of at least about 40 percent.

7. The zeolite synthesis method of claim 6 , wherein the overall relative yield on silica is at least 75%.

8. The zeolite synthesis method of claim 6 , wherein the overall relative yield on silica is at least 90%.

9. The zeolite synthesis method of claim 6 , wherein the overall relative yield on structure directing agent is at least 60%.

10. The zeolite synthesis method of claim 6 , wherein the overall relative yield on structure directing agent is at least 80%.

11. The method of claim 10 , wherein the admixture is substantially free of fluorine, fluorine ions, and fluorine containing compounds.

12. A method for achieving a high overall relative yield on silica in an AEI zeolite synthesis process comprising:
a. preparing an admixture comprising (a) at least one source of aluminum, (b) at least one source of silica, (c) at least one source of hydroxide ions, and (d) an AEI structured directing agent (SDA); wherein the structure directing agent is one or more cations selected from N,N-Dimethyl-3,5-dimethylpiperidinium, N,N-Dimethyl-2-(2-hydroxyethyl)piperidinium, N,N-Dimethyl-2-ethylpiperidinium, and 2,2,4,6,6-Pentamethyl-2-azoniabycyclo[3.2.1]octane, a mother liquor, or portion thereof, from an AEI synthesis process, and
b. reacting the admixture under crystallization conditions to form zeolite crystals having an AEI framework with a silica-to-alumina ratio (SAR) of about 8 to about 50, and a mother liquor, wherein the reacting results in an overall relative yield on silica of at least about 60 percent.

13. A composition comprising aluminosilicate AEI zeolite crystals having a mean aspect ratio (L/D) of less than or equal to about 3.

14. The composition of claim 13 , wherein the aluminosilicate zeolite has a silica-to-alumina ratio of about 15 to about 35.

15. The composition of claim 14 , wherein the aluminosilicate zeolite contains post-synthesis exchanged ions of one or more transition metals.

16. The composition of claim 14 , wherein the aluminosilicate zeolite contains about 0.5 to 5 weight percent post-synthesis exchanged copper ions, based on the total weight of the zeolite.

Assignees

• Johnson Matthey Plc

Inventors

• Yang Sanyuan
• Casci John Leonello
• Lang David

Classifications

• C01B39/48 Primary

  using at least one organic template directing agent · CPC title

• C01B39/04 Primary

  using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound · CPC title

• B01J29/70 Primary

  of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 · CPC title

• C01B39/46

  Other types characterised by their X-ray diffraction pattern and their defined composition {(C01B39/023, C01B39/026, C01B39/06 take precedence)} · CPC title

• B01J29/78

  containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium · CPC title