Hierarchical zeolites and preparation method therefor

Patent metadata

Field	Value
Publication number	US-11434140-B2
Application number	US-201917277822-A
Country	US
Kind code	B2
Filing date	Sep 20, 2019
Priority date	Sep 21, 2018
Publication date	Sep 6, 2022
Grant date	Sep 6, 2022

Abstract

The present invention relates to a method for preparing hierarchical zeolites, including the steps of preparing a first mixture solution including a structure-directing agent, an alumina precursor and a pH controller; preparing a second mixture solution by injecting a silica precursor into the first mixture solution; preparing an aqueous solution including a surfactant; preparing a third mixture solution by injecting the aqueous solution into the second mixture solution; and drying and heat-treating the third mixture solution. According to the present invention, hierarchical zeolites having a uniform morphology can be prepared, and thus hierarchical zeolites having improved activity are provided.

First claim

The invention claimed is:

1. A method for preparing a hierarchical zeolite, comprising:
preparing a first mixture solution containing a structure-directing agent having a carbon number of C10 or less and an ammonium functional group, an alumina precursor, and a pH adjusting material;
adding a silica precursor to the first mixture solution to prepare a second mixture solution;
preparing an aqueous solution containing a surfactant having a carbon number of C11 or more and an ammonium function group;
adding the aqueous solution to the second mixture solution to prepare a third mixture solution; and
hydrothermal reaction and drying of the third mixture solution,
wherein the structure-directing agent is added in a molar ratio of 1/120 to 1/50, relative to an amount of silica,
wherein the surfactant is added in a molar ratio of 1/200 to 1/50, relative to an amount of silica,
wherein a concentration of the surfactant in the aqueous solution is 77 mmol/L to 360 mmol/L, and
wherein the hierarchical zeolite is ZSM-48.

2. The method of claim 1 , wherein the structure-directing agent is at least one selected from the group consisting of tetramethylammonium bromide, tetramethylammonium chloride, tetramethylammonium hydroxide, tetraethylammonium bromide, tetraethylammonium chloride, tetraethylammonium hydroxide, tetraethylammonium tetrafluoroborate, hexamethonium chloride, and hexamethonium bromide.

3. The method of claim 1 , wherein the surfactant is at least one selected from the group consisting of cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, and cetylpyridinium chloride.

4. The method of claim 1 , wherein the preparing a third mixture solution comprises adding the aqueous solution to the second mixture solution in a dropwise manner.

5. The method of claim 1 , wherein the method is performed, without containing a seed.

6. The method of claim 1 ,
wherein the structure-directing agent is at least one selected from the group consisting of hexamethonium chloride and hexamethonium bromide;
wherein the surfactant is at least one selected from the group consisting of cetyltrimethylammonium chloride, cetyltrimethylammonium bromide, and cetylpyridinium chloride;
wherein the structure-directing agent is added in a molar ratio of 1/120 to 1/50, relative to an amount of silica;
wherein the surfactant is added in a molar ratio of 1/200 to 1/50, relative to an amount of silica; and
wherein a concentration of the surfactant in the aqueous solution is 77 mmol/L to 360 mmol/L.

Assignees

• Sk Innovation Co Ltd
• Sk Lubricants Co Ltd

Inventors

• Lim Seon-Ju
• Kim Tae-Jin
• Cheon Young-Eun

Classifications

• C01B39/04 Primary

  using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound · CPC title

• C01B39/48

  using at least one organic template directing agent · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title