# US 10,118,163 B1 · Methods for producing hierarchical mesoporous zeolite beta

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- Number: US 10,118,163 B1
- Document ID: US10118163B1
- Status: Granted
- Kind: B1
- Application number: 15/662,756
- Filed: 2017-07-28
- Granted: 2018-11-06
- Earliest claimed: 2017-07-28
- Assignees: Saudi Arabian Oil Company
- Applicants: Saudi Arabian Oil Company
- Inventors: Ke Zhang
- Web page: https://patentgrep.com/patent/US10118163B1

## CPC

- B01J 29/7007: {Zeolite Beta}
- B01J 35/633: {less than 0.5 ml/g}
- B01J 35/647: {2-50 nm}
- B01J 35/69: bimodal
- B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/10: in the presence of water, e.g. steam
- C01B 39/026: {After-treatment}
- C01B 39/46: Other types characterised by their X-ray diffraction pattern and their defined composition {(C01B39/023, C01B39/026, C01B39/06 take precedence)}
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2006/14: Pore volume
- C01P 2006/16: Pore diameter
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Embodiments of the present disclosure are directed to a method of producing hierarchical mesoporous zeolite beta. The method comprises providing a parent zeolite beta with a silicon to aluminum molar ratio of 5 to 50. The method further comprises, mixing the parent zeolite beta with an aqueous metal hydroxide solution and heating the parent zeolite beta and aqueous metal hydroxide mixture to a temperatures greater than or equal to 100° C. to produce the hierarchical mesoporous beta zeolites having and average pore size greater than 8 nm. In embodiments, the hierarchical mesoporous beta zeolites are produced without a templating agent or pore-directing agent.

## Claims

### Claim 1

A method for producing hierarchical mesoporous beta zeolites comprising:
providing parent beta zeolites having a molar ratio of silicon to aluminum of from 5 to 50;
mixing the parent beta zeolites with an aqueous metal hydroxide solution, where the aqueous metal hydroxide is an alkali metal hydroxide or an alkali earth metal hydroxide, or both; and
heating the parent beta zeolites and aqueous metal hydroxide mixture at an autogenous pressure to a temperature greater than or equal to 100° C. to produce the hierarchical mesoporous beta zeolites having an average pore size greater than 8 nanometers;
where the hierarchical mesoporous beta zeolites are produced without a templating agent or a pore-directing agent; and
where the produced hierarchical mesoporous beta zeolites have a total pore volume greater than or equal to 0.30 cm3/g.

### Claim 2 (depends on 1)

A method of claim 1, where the parent beta zeolites have a molar ratio of silicon to aluminum of from 10 to 25.

### Claim 3 (depends on 1)

A method of claim 1, where the parent beta zeolite and aqueous metal hydroxide mixture is heated to a temperature greater than 100° C.

### Claim 4 (depends on 1)

A method of claim 1, where the parent beta zeolite and aqueous metal hydroxide mixture is heated for a time interval of greater than or equal to 1 hour.

### Claim 5 (depends on 1)

A method of claim 1, where the produced hierarchical mesoporous beta zeolites exhibit an x-ray diffraction peak at 2Θ from 7 degrees to 9 degrees and another x-ray diffraction peak at 2Θ from 21 degrees to 23 degrees.

### Claim 6 (depends on 1)

A method of claim 1, where the produced hierarchical mesoporous beta zeolites have a peak pore size of greater than or equal to 20 nanometers.

### Claim 7 (depends on 1)

A method of claim 1, where the pH of the parent beta zeolites and aqueous metal hydroxide mixture is greater than or equal to 12.

### Claim 8 (depends on 1)

A method of claim 1, where the concentration of the aqueous metal hydroxide solution has a concentration from 0.01 M to 10 M.