IP Library Granted Patent US 10,213,748
Granted Patent B2
US 10,213,748 · App. 15/386,217 · Granted Feb 26, 2019

Pore opened zeolite nanosheets and their suspensions and methods and uses related thereto

Inventors: Michael Tsapatsis (Edina, MN); Qiang Xiao (Minneapolis, MN); Han Zhang (Minneapolis, MN)
Assignee: Regents of the University of Minnesota
B01D71/028B01D53/228B01D67/0039B01D67/0051B01J29/06B01J29/40B01J29/70B01J29/7038B01J35/0006B01J35/023B01J35/065B01J35/10B01J37/0246B01J37/04B01J37/343C01B39/026C01B39/48B01D2256/24B01D2257/7022B01J37/12B01J2229/10B01J2229/22B01J2229/30B01J2229/37
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Quick Facts
Patent No.
US 10,213,748
App. No.
15/386,217
Granted
Feb 26, 2019
Kind
B2
Abstract

Methods for forming two-dimensional (2D) zeolite nanosheets include exposing a multi-lamellar (ML) zeolite material including an organic structure directing agent (OSDA) to a mixture including sulfuric acid and hydrogen peroxide under conditions sufficient to remove substantially all of the OSDA from the ML zeolite material; and after exposing the ML zeolite material, treating a solution containing the ML zeolite material to sonication and/or mixing under conditions sufficient to substantially exfoliate layers of the ML zeolite to obtain porous two-dimensional zeolite nanosheets that are substantially free of the OSDA. In some cases, without further treatment such as secondary growth of the zeolite coating layer, a deposit of the OSDA-free nanosheets on polymer support exhibits hydrocarbon isomer selectivity.

Claims (25)

1. A method, comprising:

exposing a multi-lamellar (ML) zeolite material comprising an organic structure directing agent (OSDA) to a mixture comprising sulfuric acid and hydrogen peroxide under conditions sufficient to remove substantially all of the OSDA from the ML zeolite material; and

after exposing the ML zeolite material, treating a solution containing the ML zeolite material to sonication and/or mixing under conditions sufficient to substantially exfoliate layers of the ML zeolite to obtain porous two-dimensional zeolite nanosheets that are substantially free of the OSDA.

2. The method of claim 1 , wherein the ML zeolite material comprises an WI zeolite.

3. The method of claim 1 , wherein the ML zeolite material comprises an MWW zeolite.

4. The method of claim 1 , wherein the mixture comprises at least 2.5 parts sulfuric acid to 1 part hydrogen peroxide by volume.

5. The method of claim 4 , wherein the mixture comprises no more than 7 parts sulfuric acid to 1 part hydrogen peroxide by volume.

6. The method of claim 1 , wherein exposing the ML zeolite material comprises providing the ML zeolite material in the sulfuric acid and adding the hydrogen peroxide to the sulfuric acid or by preparing a mixture of sulfuric acid and hydrogen peroxide and adding the ML zeolite to the mixture.

7. The method of claim 1 , further comprising synthesizing the ML zeolite material using the OSDA prior to exposing the ML zeolite material.

8. The method of claim 1 , wherein the ML zeolite material is exposed to the mixture for a time sufficient to remove the OSDA to a desired level.

9. The method of claim 1 , wherein the ML zeolite material is exposed to mixtures comprising sulfuric acid and hydrogen peroxide multiple times to remove substantially all of the OSDA from the ML zeolite material.

10. The method of claim 1 , wherein the sonication or mixing is performed by a technique selected from the group consisting of bath sonication, horn sonication, vortexing, and shaking including combinations of them.

11. The method of claim 1 , wherein the solution containing the ML zeolite material is an aqueous solution.

12. A method of forming a zeolite membrane, comprising:

obtaining porous two-dimensional zeolite nanosheets using the method of claim 1 ; and

forming the zeolite membrane using the porous two-dimensional zeolite nanosheets.

13. A method, comprising:

exposing a zeolite nanosheet material comprising an organic structure directing agent (OSDA) to a mixture comprising sulfuric acid and hydrogen peroxide under conditions sufficient to remove substantially all of the OSDA from the zeolite nanosheet material; and

after exposing the zeolite nanosheet material, dispersing it in a polar solvent.

14. The method of claim 13 , where the polar solvent is water.

15. The method of claim 13 , further comprising, prior to exposing the zeolite nanosheet material to the mixture, exfoliating a ML zeolite material to provide the zeolite nanosheet material.

16. The method of claim 15 , wherein the ML zeolite material is exfoliated by melt blending.

17. A method of forming a zeolite membrane, comprising:

obtaining porous two-dimensional zeolite nanosheets using the method of claim 13 ; and

forming the zeolite membrane using the porous two-dimensional zeolite nanosheets.

Assignments (2)
CONFIRMATORY LICENSE Recorded Nov 28, 2023
From: REGENTS OF THE UNIVERSITY OF MINNESOTA
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 065681/0577 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 29, 2020
From: TSAPATSIS, MICHAEL; XIAO, QIANG; ZHANG, HAN
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 053920/0090 →
Continuity (2)
Provisional Application 62270134 · Dec 21, 2015
Related Publication 20170173539A1 · Jun 22, 2017