US 12,434,974 B2
Synthesis of finned zeolite crystals
Jeffrey D. Rimer, Houston, TX (US); Yufeng Shen, Columbia, MD (US); and Heng Dai, Houston, TX (US)
Assigned to UNIVERSITY OF HOUSTON SYSTEM, Houston, TX (US)
Appl. No. 17/798,748
Filed by University of Houston System, Houston, TX (US)
PCT Filed Feb. 9, 2021, PCT No. PCT/US2021/017188
§ 371(c)(1), (2) Date Aug. 10, 2022,
PCT Pub. No. WO2021/163021, PCT Pub. Date Aug. 19, 2021.
Claims priority of provisional application 62/975,254, filed on Feb. 12, 2020.
Prior Publication US 2023/0077288 A1, Mar. 9, 2023
Int. Cl. C01B 39/02 (2006.01); C01B 39/40 (2006.01); C01B 39/44 (2006.01); C01B 39/48 (2006.01)
CPC C01B 39/026 (2013.01) [C01B 39/40 (2013.01); C01B 39/445 (2013.01); C01B 39/48 (2013.01); C01P 2004/90 (2013.01)] 10 Claims
OG exemplary drawing
 
1. A method for preparing finned zeolite crystals, comprising:
preparing a secondary growth solution for epitaxial growth of finned protrusions from zeolite seed crystals, wherein the secondary growth solution comprises framework source precursors, one or more structure-directing agents, and a hydroxide source, wherein the framework source precursors comprise a silica source and an alumina source;
adding the zeolite seed crystals in an amount of about 5 to about 30 weight percent of the secondary growth solution to produce a seeded growth solution for post-synthesis modification of the zeolite seed crystals;
heating the seeded growth solution to a temperature of about 100° C. to about 170° C. for about 6 to about 48 hours, to produce epitaxially grown fins on the zeolite seed crystals in the seeded growth solution;
quenching the seeded growth solution to room temperature to produce a final growth solution; and
isolating finned zeolite crystals from the final growth solution, wherein the finned zeolite crystals comprise a zeolite seed crystal portion and a plurality of epitaxially grown fins extending from outer surfaces of the zeolite seed crystal portion, wherein the zeolite seed crystal portion comprises the zeolite seed crystals from the seeded growth solution, wherein the zeolite seed crystal portion has a characteristic size of β, wherein the epitaxially grown fins have a characteristic size of α, wherein β is greater than α, wherein a is less than about 50 nm, wherein the zeolite seed crystal portion comprises a single crystallographic registry, wherein the zeolite seed crystal portion comprises a network of pores, wherein the epitaxially grown fins comprise a single crystallographic registry that is identical to the single crystallographic registry of the zeolite seed crystal portion, and wherein the epitaxially grown fins comprise a network of pores that is continuous with the network of pores of the zeolite seed crystal portion.