IP Library Granted Patent US 11,014,821
Granted Patent B2
US 11,014,821 · App. 16/506,253 · Granted May 25, 2021

Methods for preparation of CHA Zeolite at ambient pressure

Inventor: David Ari Lang (Longwood, FL)
Assignee: Zeolyfe, LLC
C01B39/48B01J29/7015B01J19/18B01J2219/0013B01J2219/00101
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 11,014,821
App. No.
16/506,253
Granted
May 25, 2021
Kind
B2
Abstract

The disclosure, in one aspect, relates to methods of preparing a CHA zeolite under ambient pressure conditions. In further aspects, the disclosure relates to methods such that a mother liquor can be isolated from a disclosed method, and recycled for use in a disclosed method for further preparation of a CHA zeolite. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present disclosure.

Claims (29)

1. A method for preparing a CHA zeolite, the method comprising:

heating a zeolite precursor mixture at ambient pressure under reflux conditions;

wherein the zeolite precursor mixture comprises water, a silicate solution, a zeolite, and a CHA templating agent;

wherein heating comprises heating such that the zeolite precursor mixture has a reaction temperature of from about 80° C. to about 120° C.;

thereby forming a CHA zeolite and a mother liquor solution.

2. The method of claim 1 , wherein the ambient pressure is about 700 torr to about 800 torr.

3. The method of claim 1 , wherein the zeolite in the zeolite precursor mixture is selected from a USY zeolite, heat-treated Na—Y zeolite, a Na—Y zeolite, and combinations thereof.

4. The method of claim 3 , wherein the zeolite in the zeolite precursor mixture is selected from a heat-treated Na—Y zeolite, a Na—Y zeolite, and combinations thereof.

5. The method of claim 3 , wherein the zeolite in the zeolite precursor mixture is selected from a USY zeolite.

6. The method of claim 1 , wherein the silicate solution in the zeolite precursor mixture is a sodium silicate solution comprising SiO 2 Na 2 O, and water.

7. The method of claim 1 , wherein the CHA templating agent is selected from N, N, N-trimethyl-1-ammonium adamantine, tetraethylenepentamine, and a combination thereof.

8. The method of claim 1 , wherein heating further comprises heating such that an internal portion proximal to a top end of a reflux condenser containing reaction contents has a temperature of about 30° C. to about 70° C.

9. The method of claim 1 , wherein the heating is carried out for a period of time of about 12 hours to about 96 hours.

10. The method of claim 1 , further comprising terminating the heating; cooling the contents of the reaction to an ambient temperature; separating the CHA zeolite from the liquid mixture; wherein the liquid mixture separated from the CHA zeolite is a mother liquor solution comprising SiO 2 , Na 2 O, and water.

11. The method of claim 1 , wherein the zeolite precursor mixture has a ratio of H 2 O to Al 2 O 3 of about 400 to about 1000.

12. A method for preparing a CHA zeolite, the method comprising:

mixing a mother liquor solution isolated from the reaction of claim 1 with a zeolite precursor mixture comprising a silicate solution, a zeolite, and a CHA templating agent;

heating the mother liquor solution and the zeolite precursor mixture at ambient pressure under reflux conditions;

wherein the mother liquor solution comprises SiO 2 , Na 2 O, and water;

wherein heating comprises heating such that the zeolite precursor mixture and the mother liquor solution has a reaction temperature of from about 80° C. to about 120° C.; and

thereby forming a CHA zeolite and a secondary mother liquor solution.

13. The method of claim 12 , wherein the ambient pressure is about 700 torr to about 800 torr.

14. The method of claim 12 , wherein the zeolite in the zeolite precursor mixture is selected from a USY zeolite, a heat-treated Na—Y zeolite, a Na—Y zeolite, and combinations thereof.

15. The method of claim 14 , wherein the zeolite in the zeolite precursor mixture is selected from a heat-treated Na—Y zeolite, a Na—Y zeolite, and combinations thereof.

16. The method of claim 14 , wherein the zeolite in the zeolite precursor mixture is a USY zeolite.

17. The method of claim 12 , wherein the CHA templating agent in the zeolite precursor mixture is N,N,N-trimethyl-1-ammonium adamantine.

18. The method of claim 12 , wherein heating further comprises heating such that an internal portion proximal to a top end of a reflux condenser containing reaction contents has a temperature of about 30° C. to about 70° C.

19. The method of claim 12 , wherein the heating is carried out for a period of time of about 12 hours to about 96 hours.

20. The method of claim 12 , wherein the CHA templating agent is selected from N, N, N-trimethyl-1-ammonium adamantine, tetraethylenepentamine, and a combination thereof.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 28, 2024
From: ZEOLYFE LABS INC
To: SITHAMBARAM, SHANTHAKUMAR
Reel/Frame 069035/0717 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 3, 2022
From: ZEOLYFE, LLC
To: ZEOLYFE LABS INC
Reel/Frame 060095/0795 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 20, 2019
From: LANG, DAVID ARI
To: ZEOLYFE, LLC
Reel/Frame 050097/0815 →
Continuity (2)
Provisional Application 62695269 · Jul 9, 2018
Related Publication 20200010332A1 · Jan 9, 2020