US 12,011,711 B1
Method for synthesizing mesoporous nano-sized ultra-stable Y zeolite
Faisal Alotaibi, Al Khobar (SA); and Lianhui Ding, Dhahran (SA)
Assigned to Saudi Arabian Oil Company, Dhahran (SA)
Filed by Saudi Arabian Oil Company, Dhahran (SA)
Filed on Nov. 29, 2022, as Appl. No. 18/059,728.
This patent is subject to a terminal disclaimer.
Int. Cl. B01J 29/08 (2006.01); B01J 35/23 (2024.01); B01J 35/50 (2024.01); B01J 35/61 (2024.01); B01J 35/63 (2024.01); B01J 35/64 (2024.01); B01J 37/00 (2006.01); B01J 37/03 (2006.01); B01J 37/04 (2006.01); B01J 37/06 (2006.01); B01J 37/08 (2006.01); B01J 37/30 (2006.01); C01B 39/08 (2006.01); C01B 39/24 (2006.01)
CPC B01J 29/084 (2013.01) [B01J 35/23 (2024.01); B01J 35/50 (2024.01); B01J 35/617 (2024.01); B01J 35/633 (2024.01); B01J 35/635 (2024.01); B01J 35/647 (2024.01); B01J 37/009 (2013.01); B01J 37/036 (2013.01); B01J 37/04 (2013.01); B01J 37/06 (2013.01); B01J 37/08 (2013.01); B01J 37/30 (2013.01); C01B 39/08 (2013.01); C01B 39/24 (2013.01); B01J 2229/16 (2013.01); B01J 2229/32 (2013.01); C01P 2004/03 (2013.01); C01P 2004/62 (2013.01); C01P 2004/64 (2013.01); C01P 2006/12 (2013.01); C01P 2006/14 (2013.01); C01P 2006/16 (2013.01)] 16 Claims
 
1. A method for synthesizing a mesoporous nano-sized ultra-stable Y zeolite, the method comprising:
mixing sodium hydroxide and water to form an aqueous NaOH solution;
adding sodium aluminate and colloidal silica to the aqueous NaOH solution and mixing to form a hydrogel, where the hydrogel has a molar ratio composition of 5 to 15 Na2O:Al2O3:7 to 20 SiO2:200 to 400 H2O;
transferring the hydrogel to an autoclave operated at 50° C. to 70° C. for 10 to 20 hours;
further operating the autoclave at 80° C. to 120° C. for 10 to 20 hours to form a zeolite precursor;
filtering and washing the zeolite precursor with water until the pH reaches 8 to 9 to form a nano-sized Y zeolite;
combining the nano-sized Y zeolite with 30 to 1,000 milliliters water per gram of the nano-sized Y zeolite on a dry basis to form a nano-sized Y zeolite slurry mixture and heating the nano-sized Y zeolite slurry mixture to 70° C. to 100° C.;
adding a 0.1 to 2.0 M aqueous solution of ammonium hexafluorosilicate over 1 to 2 hours to the nano-sized Y zeolite slurry mixture to form a dealuminated solution;
holding the dealuminated solution at 70° C. to 100° C. for 1 to 8 hours;
filtering and washing the dealuminated solution with water to form an ultra-stable Y zeolite precursor;
drying the ultra-stable Y zeolite precursor at 80° C. to 150° C. for 6 to 24 hours to form a dried zeolite precursor; and
calcining the dried zeolite precursor at 250° C. to 600° C. for 1 to 8 hours to form the nano-sized ultra-stable Y zeolite.