US 12,391,561 B2
Method to lower structure directing agent content requirement for manufacture of crystalline material having a CHA framework
Robert Peter Hodgkins, Dhahran (SA); Omer Refa Koseoglu, Dhahran (SA); Javier Ruiz Martinez, Thuwal (SA); and Moussa Zaarour, Thuwal (SA)
Assigned to Saudi Arabian Oil Company, Dhahran (SA)
Filed by Saudi Arabian Oil Company, Dhahran (SA)
Filed on Jan. 10, 2023, as Appl. No. 18/152,484.
Prior Publication US 2024/0239672 A1, Jul. 18, 2024
This patent is subject to a terminal disclaimer.
Int. Cl. C01B 39/48 (2006.01)
CPC C01B 39/48 (2013.01) [C01P 2002/72 (2013.01); C01P 2002/86 (2013.01); C01P 2002/88 (2013.01)] 21 Claims
OG exemplary drawing
 
1. A method for synthesis of CHA framework crystalline material comprising:
forming a homogeneous aqueous mixture of a silica source, a framework metal oxide source selected from compounds of Al, Fe, B and Ga, an alkali metal source, a structure directing agent, water and an effective amount of water-soluble oxidized disulfide oil (ODSO), wherein the amount of structure directing agent is less than or equal to an amount of structure directing agent of a baseline homogeneous aqueous mixture in the absence of ODSO, and wherein the baseline homogeneous aqueous mixture is formed of, relative to the homogeneous aqueous mixture including ODSO, an approximately equivalent composition of the silica source, the framework metal oxide source and the alkali metal source, except for an amount of water instead of the ODSO, and wherein the amount of the structure directing agent in the baseline homogeneous aqueous mixture is greater than or equal to the amount of the structure directing agent in the homogeneous aqueous mixture; and
heating the homogeneous aqueous mixture under conditions and for a time effective to form a precipitate suspended in a supernatant as an intermediate suspension, wherein the precipitate comprises CHA framework crystalline material, wherein CHA framework crystalline material uptakes structure directing agent into pores of the CHA framework crystalline material during formation, and wherein an amount of structure directing agent uptake during formation is less than or equal to an amount of structure directing agent uptake into pores during synthesis of a baseline precipitate from the baseline homogeneous aqueous mixture in the absence of ODSO under approximately equivalent heat and time as that applied to the homogeneous aqueous mixture,
wherein the precipitate contains an amount of CHA framework crystalline material that is greater than or equal to an amount of crystalline material having a CHA framework contained in the baseline precipitate.