Synthesis of finned zeolite crystals

Patent metadata

Field	Value
Publication number	US-12434974-B2
Application number	US-202117798748-A
Country	US
Kind code	B2
Filing date	Feb 9, 2021
Priority date	Feb 12, 2020
Publication date	Oct 7, 2025
Grant date	Oct 7, 2025

Abstract

A secondary growth procedure described herein is used to prepare finned zeolites. The finned zeolites possess properties that are distinctly unique compared to crystals of similar size lacking fins. The procedure is amenable to a wide range of zeolite crystal structures.

First claim

What is claimed is:

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.

2. The method of claim 1 , wherein the framework source precursors comprise sodium silicate, tetraethylorthosilicate, colloidal silicate, fumed silica, SiO 2 , aluminum sulfate, aluminum hydroxide, Al 2 O 3 , or combinations thereof.

3. The method of claim 1 , wherein the one or more structure-directing agents are inorganic, organic, or a combination thereof.

4. The method of claim 1 , wherein the one or more structure-directing agents are selected from pyrrolidine, tetrapropylammonium hydroxide, 1,8-diaminooctane, cyclohexylamine and tetrabutylammonium hydroxide.

5. The method of claim 1 , wherein the hydroxide source is Na 2 O or K 2 O.

6. The method of claim 1 , wherein the secondary growth solution has a molar composition ratio of a first framework source precursor to a second framework source precursor of about 40:1 to about 120:1, and wherein the first framework source precursor is SiO 2 and the second framework source precursor is Al 2 O 3 .

7. The method of claim 1 , wherein the secondary growth solution has a molar composition ratio of the framework source percursors to the one or more structure-directing agents of about 2:1 to about 15:1.

8. The method of claim 1 , wherein the secondary growth solution has a molar composition ratio of the framework source percursors to the hydroxide source of about 8:1 to about 65:1.

9. The method of claim 1 , wherein the finned zeolite crystals are MEL type, MFI type, or FER type.

10. The finned zeolite crystals prepared by the method of claim 1 .

Assignees

• Univ Houston System

Inventors

• Rimer Jeffrey D
• Shen Yufeng
• Dai Heng

Classifications

• C01P2004/90

  Other morphology not specified above · CPC title

• C01B39/48

  using at least one organic template directing agent · CPC title

• C01B39/445

  using at least one organic template directing agent · CPC title

• C01B39/40

  using at least one organic template directing agent · CPC title

• C01B39/02

  Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof · CPC title