Novel zeolite synthesis with a fluoride source
US-2018093255-A1 · Apr 5, 2018 · US
US11826737B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11826737-B2 |
| Application number | US-202117559732-A |
| Country | US |
| Kind code | B2 |
| Filing date | Dec 22, 2021 |
| Priority date | Sep 9, 2019 |
| Publication date | Nov 28, 2023 |
| Grant date | Nov 28, 2023 |
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Disclosed is a method of preparing a high-performance zeolite catalyst for reducing nitrogen oxide emissions, and more particularly a technique for preparing a zeolite catalyst, suitable for use in effectively removing nitrogen oxide (NOx), among exhaust gases emitted from vehicle internal combustion engines through selective catalytic reduction (SCR), thereby exhibiting high efficiency, high chemical stability and high thermal durability upon SCR using the prepared catalyst.
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What is claimed is: 1. A method of preparing a copper-impregnated LTA zeolite catalyst, the method comprising: producing an LTA zeolite, wherein the producing of the LTA zeolite is performed using a fluorine-substituted structure-directing agent (SDA-F) that is subjected to mixing with a silicon material, an aluminum material, and a template, and then to a hydrothermal synthesis that is performed through a two-stage temperature-elevating synthesis process, and impregnating copper in the LTA zeolite, wherein the two-stage temperature-elevating synthesis process is performed at 100° C. to 120° C. for 5 to 10 hours, and then the temperature is raised to 150° C. to 200° C. for 10 to 15 hours. 2. The method of claim 1 , wherein the fluorine-substituted structure-directing agent is a fluorine-substituted imidazole-based cation material. 3. The method of claim 1 , wherein the fluorine-substituted structure-directing agent is produced by substituting a structure-directing agent through linking with a fluorine-containing ion exchange resin or addition of a fluorine source. 4. The method of claim 3 , wherein the fluorine source is selected from the group consisting of hydrogen fluoride, ammonium fluoride, sodium fluoride, potassium fluoride, and alkylammonium fluoride. 5. The method of claim 1 , wherein a seed crystal introduction is further performed between the mixing and the hydrothermal synthesis. 6. The method of claim 1 , wherein the hydrothermal synthesis is performed at a water/silicon (H 2 O/Si) molar ratio of 2.5 to 20. 7. The method of claim 1 , wherein the silicon material is selected from the group consisting of ammonia (NH 4 )-colloidal silica, sodium (Na)-colloidal silica, precipitated silica, fumed silica, sodium silicate, tetraethyl orthosilicate, and aluminosilicate. 8. The method of claim 7 , wherein the ammonia-colloidal silica is used such that a state of a synthetic mother liquor is maintained in a liquid phase. 9. The method of claim 1 , wherein the aluminum material is selected from the group consisting of aluminum sulfate, crystalline aluminum hydroxide, noncrystalline aluminum hydroxide, aluminum chloride, aluminosilicate, and aluminum metal. 10. The method of claim 1 , wherein a copper source used in the impregnating of the copper is selected from the group consisting of copper nitrate, copper chloride, copper acetate, and an amine-based precursor including tetraammine copper nitrate, tetraammine copper chloride and tetraammine copper sulfate. 11. The method of claim 10 , wherein the LTA zeolite is impregnated 1 to 3 times using the copper source. 12. The method of claim 1 , wherein the template is selected from the group consisting of tetramethylammonium hydroxide and tetramethylammonium chloride. 13. The method of claim 5 , wherein the seed crystal introduction is performed using an LTA-structured zeolite having a Si/Al molar ratio of 10-20, in which an amount of a seed crystal introduced relative to the silicon material is 1-5 wt %.
Hydropyrolysis · CPC title
characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77) · CPC title
A-type · CPC title
X-ray diffraction · CPC title
Scanning electron microscopy; Transmission electron microscopy · CPC title
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