SDA-free synthesis of chabazite (CHA) zeolite and uses thereof

Patent metadata

Field	Value
Publication number	US-11247911-B2
Application number	US-201915733504-A
Country	US
Kind code	B2
Filing date	Apr 22, 2019
Priority date	May 3, 2018
Publication date	Feb 15, 2022
Grant date	Feb 15, 2022

Abstract

A method of making a chabazite zeolite is disclosed. The method can include obtaining an aqueous gel comprising silicon dioxide, aluminum oxide, potassium oxide, and a nucleating agent, and hydrothermally treating the aqueous gel to obtain the chabazite zeolite.

First claim

The invention claimed is:

1. A method of making a chabazite zeolite, the method comprising:
(a) obtaining an aqueous gel comprising silicon dioxide (SiO 2 ), aluminum oxide (Al 2 O 3 ), potassium oxide (K 2 O), and a nucleating agent; and
(b) hydrothermally treating the aqueous gel to obtain the chabazite zeolite;
wherein the chabazite zeolite is calcined;
wherein the chabazite zeolite is in the form of cuboid particles;
and
wherein the aqueous gel has a molar composition of:
1SiO 2 :0.2Al 2 O 3 :0.39K 2 O:0.3NH 4 F:xH 2 O, where x is the molar ratio of H 2 O/SiO 2 and ranges from 10 to 15.

2. The method of claim 1 , wherein the aqueous gel in step (a) is maintained at room temperature for 12 to 24 hours prior to the step (b) hydrothermal treatment.

3. The method of claim 2 , wherein the cuboid particles have a particle size of 1.2 to 2 μm.

4. The method of claim 1 , wherein x is 15.

5. The method of claim 4 , wherein the cuboid particles have a particle size of 1.2 to 2 μm.

6. The method of claim 1 , wherein x is 10.

7. The method of claim 1 , wherein the gel further comprises Na 2 O.

8. The method of claim 1 , wherein hydrothermal treatment is performed at a temperature of 130° C.

9. The method of claim 8 , wherein the cuboid particles have a particle size of 1.2 to 2 μm.

10. The method of claim 1 , further comprising:
(c) washing the chabazite zeolite until a pH of about 7 is obtained; and
(d) performing an ion-exchange to protonate the chabazite zeolite to produce an H-form of the chabazite zeolite.

11. The method of claim 1 , wherein the aqueous gel from step (a) is obtained by:
(i) forming an aqueous solution comprising aluminum hydroxide and potassium hydroxide; and
(ii) adding ammonium fluoride and colloidal silica to the aqueous solution to form the aqueous gel.

12. The method of claim 1 , wherein a templating agent is not used to produce the chabazite zeolite.

13. The method of claim 1 , wherein the templating agent is N,N,N-trimethyl-1-adamantammonium iodide.

14. The method of claim 1 , wherein the hydrothermal treatment is performed in a PTFE-lined stainless-steel autoclave.

15. The method of claim 1 , wherein the cuboid particles have a particle size of 1.2 to 2 μm.

16. The method of claim 15 , wherein the cuboid particles are agglomerated to form large interconnected particles ranging in size from 15 to 20 μm.

17. The method of claim 1 , wherein the cuboid particles have a particle size of 1.2 μm.

18. A method of making a chabazite zeolite, the method consisting of the steps of:
(a) obtaining an aqueous gel comprising silicon dioxide (SiO 2 ), aluminum oxide (Al 2 O 3 ), potassium oxide (K 2 O), and a nucleating agent; and
(b) hydrothermally treating the aqueous gel to obtain the chabazite zeolite;
wherein the chabazite zeolite is calcined;
wherein the aqueous gel has a molar composition of:
1SiO 2 :0.2Al 2 O 3 :0.39K 2 O:0.3NH 4 F:xH 2 O, where x is the molar ratio of H 2 O/SiO 2 and ranges from 10 to 15;
wherein the cuboid particles are agglomerated to form large interconnected particles ranging in size from 15 to 20 μm, and
wherein the cuboid particles have a have a particle size of 1.2 to 2 μm.

19. A method of making a chabazite zeolite, the method consisting of the steps of:
(a) obtaining an aqueous gel comprising silicon dioxide (SiO 2 ), aluminum oxide (Al 2 O 3 ), potassium oxide (K 2 O), and a nucleating agent; and
(b) hydrothermally treating the aqueous gel to obtain the chabazite zeolite;
wherein the chabazite zeolite is calcined;
wherein the aqueous gel has a molar composition of:
1SiO 2 :0.2Al 2 O 3 :0.39K 2 O:0.3NH 4 F:xH 2 O, where x is the molar ratio of H 2 O/SiO 2 and ranges from 10 to 15;
wherein the cuboid particles are agglomerated to form large interconnected particles ranging in size from 15 to 20 μm,
wherein the cuboid particles have a have a particle size of 1.2 to 2 μm; and
wherein the chabazite zeolite further comprises sodium oxide.

Assignees

• Sabic Global Technologies Bv

Inventors

• Muraza Oki
• Nasser Galal A
• Malaibari Zuhair O
• Al Shammari Talal K
• Mayank Vyas M
• Yamani Zain

Classifications

• C01P2004/38

  cube-like · CPC title

• C01B39/46 Primary

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

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• B01J37/08

  Heat treatment {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• C01P2004/50

  Agglomerated particles · CPC title