Method for preparing mordenite zeolite having controllable particle size

Patent metadata

Field	Value
Publication number	US-11932545-B2
Application number	US-201917277811-A
Country	US
Kind code	B2
Filing date	Sep 23, 2019
Priority date	Sep 21, 2018
Publication date	Mar 19, 2024
Grant date	Mar 19, 2024

Abstract

The present disclosure relates to a method for preparing a mordenite zeolite, the method including crystallizing, at a temperature of 150° C. to 190° C., a gel which includes, in mol based on 1 mol of silica, 0.02 to 0.2 of an alumina precursor, 0.01 to 0.04 of a structure-directing agent, 0.1 to 0.18 of a pH control agent, and 10 to 100 of water. According to the present disclosure, a mordenite zeolite having high particle size uniformity and a particle size controllable while maintaining the particle size uniformity may be prepared.

First claim

The invention claimed is:

1. A method for preparing a mordenite zeolite, the method comprising crystallizing, at a temperature of 150° C. to 190° C., a gel which comprises, in mol based on 1 mol of silica, 0.02 to 0.2 of an alumina precursor, 0.01 to 0.04 of a structure-directing agent, 0.1 to 0.18 of a pH control agent, and 10 to 100 of water.

2. The method of claim 1 , wherein the gel further comprises 0.03 mol or less (excluding 0) of a surfactant based on 1 mole of silica.

3. The method of claim 1 , wherein the crystallizing is performed for 24 hours to 80 hours.

4. The method of claim 1 , wherein after the crystallizing, the mordenite zeolite has an average particle diameter within a range of 20 nm to 150 nm.

5. The method of claim 1 , wherein, to prepare the gel, the method further comprises:
dissolving the pH control agent and the silica precursor in water to provide a basic silica suspension;
dissolving the structure-directing agent and the alumina precursor in water to provide an aqueous alumina solution;
dissolving a surfactant in water to provide an aqueous surfactant solution;
providing an aqueous silica-alumina solution by mixing and agitating together the basic silica suspension and the aqueous alumina solution; and
gelation of the aqueous silica-alumina solution.

6. The method of claim 5 , wherein the gelation comprises agitation for 1 hour to 120 hours at a temperature of 20° C. to 60° C.

7. The method of claim 5 , wherein the silica precursor is added at a rate of 0.1 g/min to 1 g/min while performing agitation.

8. The method of claim 5 , wherein the structure-directing agent and the alumina precursor are individually or simultaneously added to water at a rate of 1 g/min to 10 g/min.

9. The method of claim 5 , wherein the aqueous surfactant solution is prepared by adding the surfactant to water at a temperature of 20° C. to 80° C. while performing agitation.

10. The method of claim 5 , further comprising adding the aqueous surfactant solution to the aqueous silica-alumina solution.

11. The method of claim 10 , wherein the aqueous surfactant solution is added to the silica-alumina aqueous solution at a rate of 1 cc/min to 10 cc/min.

12. The method of claim 5 , wherein the basic silica suspension is obtained by adding the pH control agent to water to prepare a basic aqueous solution, and adding the silica precursor to the basic aqueous solution to dissolve the silica precursor in the basic aqueous solution.

13. The method of claim 12 , wherein after the silica precursor is added, the silica precursor is dissolved by performing agitation for 1 to 200 hours.

14. The method of claim 5 , wherein the mixing of the basic silica suspension and the aqueous alumina solution is performed by adding the aqueous alumina solution to the basic silica suspension at a rate of 1 cc/min to 10 cc/min.

15. The method of claim 14 , wherein the mixing of the basic silica suspension and the aqueous alumina solution comprises additional agitation for 1 hour to 72 hours after the adding of the aqueous alumina solution.

Assignees

• Sk Innovation Co Ltd

Inventors

• Cheon Young-Eun
• Kim Yeon-Ho
• Lee Sang-Il
• Lee Ji-Hoon

Classifications

• C01B39/265 Primary

  using at least one organic template directing agent · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title