IP Library › Granted Patent US 12,378,130
Granted Patent B2
US 12,378,130 · App. 17/570,075 · Granted Aug 5, 2025

Methods of synthesis of mesoporous nano-sized zeolite beta by hydrothermal treatment and uses thereof

Inventors: Lianhui Ding (Dhahran Camp, SA); Sameer Al-Ghamdi (Dhahran, SA)
Assignee: Saudi Arabian Oil Company
C01B39/46C10G47/02B82Y30/00B82Y40/00C01P2004/64C01P2006/14C01P2006/16
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Quick Facts
Patent No.
US 12,378,130
App. No.
17/570,075
Granted
Aug 5, 2025
Kind
B2
Abstract

A nano-sized mesoporous zeolite beta composition and processes for the synthesis and use of the nano-sized mesoporous zeolite beta. The nano-sized mesoporous zeolite beta is synthesized using a hydrothermal treatment without drying and calcination of the zeolite prior to or after hydrothermal treatment. A process for hydrocracking a hydrocarbon feedstock using the nano-sized mesoporous zeolite beta is also provided.

Claims (29)

1. A method for synthesizing a nano-sized mesoporous zeolite beta composition, comprising:

mixing silica, a source of aluminum, tetraethylammonium hydroxide, and water to form an aluminosilicate fluid gel;

heating the aluminosilicate fluid gel at a first temperature for a first time period to form a zeolite beta product;

subjecting the zeolite beta product to a hydrothermal treatment at a pressure and second temperature for a second time period to produce the nano-sized mesoporous zeolite beta composition without the use of a structure directing agent (SDA), wherein the zeolite beta product is not dried and calcinated before the hydrothermal treatment, wherein the nano-sized mesoporous zeolite beta composition has a relative crystallinity of greater than 100%.

2. The method of claim 1 , wherein the nano-sized mesoporous zeolite beta composition has a pore volume of 1.0 milliliters per gram (ml/g) to 1.5 ml/g.

3. The method of claim 1 , wherein the nano-sized mesoporous zeolite beta composition has a pore size of 15 nanometers (nm) to 50 nm.

4. The method of claim 1 , wherein the nano-sized mesoporous zeolite beta composition has a particle size of 10 nanometers (nm) to 100 nm.

5. The method of claim 1 , wherein the silica comprises fumed silica.

6. The method of claim 1 , wherein the source of aluminum is aluminum oxide.

7. The method of claim 1 , wherein the first temperature is in the range of 100° C. to 150° C. and the first time period is in the range of 2 days to 7 days.

8. The method of claim 1 , wherein the pressure is in the range of 1 bar to 5 bar, the second temperature is in the range of 400° C. to 600° C., and the second time period is in the range of 0.5 hours to 4 hours.

9. The method of claim 1 , comprising:

filtering the nano-sized mesoporous zeolite beta composition;

washing the nano-sized mesoporous zeolite beta composition after the filtering;

drying the nano-sized mesoporous zeolite beta composition at a third temperature for a third time period after the washing; and

calcinating the nano-sized mesoporous zeolite beta composition at a fourth temperature for a fourth time period after the drying.

10. The method of claim 9 , wherein the third temperature is in the range of 80° C. to 150° C., and the third time period is in the range of 3 hours to 8 hours.

11. The method of claim 9 , wherein the fourth temperature is in the range of 500° C. to 600° C., and the fourth time period is in the range of 3 hours to 8 hours.

12. A method for hydrocracking a hydrocarbon feedstock, the method comprising:

contacting the hydrocarbon feedstock with a catalyst containing a nano-sized mesoporous zeolite beta composition under reaction conditions to convert a product stream containing at least 20 weight percent of hydrocarbons with 1 to 4 carbon atoms, wherein the nano-sized mesoporous zeolite beta composition is synthesized by a method comprising the steps of:

mixing silica, a source of aluminum, tetraethylammonium hydroxide, and water to form an aluminosilicate fluid gel;

heating the aluminosilicate fluid gel at a first temperature for a first time period to form a zeolite beta product;

subjecting the zeolite beta product to a hydrothermal treatment at a pressure and second temperature for a second time period to produce the nano-sized mesoporous zeolite beta composition without the use of a structure directing agent (SDA), wherein the zeolite beta product is not dried and calcinated before the hydrothermal treatment, wherein the nano-sized mesoporous zeolite beta composition has a relative crystallinity of greater than 100%.

13. The method of claim 12 , wherein the nano-sized mesoporous zeolite beta composition has a pore volume of 1.0 milliliters per gram (ml/g) to 1.5 ml/g, a pore size of 15 nanometers (nm) to 50 nm, and a particle size of 10 nanometers (nm) to 100 nm.

14. The method of claim 12 , wherein the silica comprises fumed silica.

15. The method of claim 12 , wherein the source of aluminum is aluminum oxide.

16. The method of claim 12 , wherein the first temperature is in the range of 100° C. to 150° C. and the first time period is in the range of 2 days to 7 days.

17. The method of claim 12 , wherein the pressure is in the range of 1 bar to 5 bar, the second temperature is in the range of 400° C. to 600° C., and the second time period is in the range of 0.5 hours to 4 hours.

18. The method of claim 12 , wherein the hydrocarbon feedstock comprises a heavy fraction comprising a boiling point greater or equal to 540° C.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 10, 2022
From: DING, LIANHUI; AL-GHAMDI, SAMEER
To: SAUDI ARABIAN OIL COMPANY
Reel/Frame 058592/0173 →
Continuity (1)
Related Publication 20230212018A1 · Jul 6, 2023
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