Iron-loaded small pore aluminosilicate zeolites and method of making metal loaded small pore aluminosilicate zeolites

Patent metadata

Field	Value
Publication number	US-11634335-B2
Application number	US-202016739615-A
Country	US
Kind code	B2
Filing date	Jan 10, 2020
Priority date	Jan 14, 2019
Publication date	Apr 25, 2023
Grant date	Apr 25, 2023

Abstract

The present invention provides an iron-loaded aluminosilicate zeolite having a maximum pore opening defined by eight tetrahedral atoms and having the framework type CHA, AEI, AFX, ERI or LTA, wherein the iron (Fe) is present in a range of from about 0.5 to about 5.0 wt. % based on the total weight of the iron-loaded aluminosilicate zeolite, wherein an ultraviolet-visible absorbance spectrum of the iron-loaded synthetic aluminosilicate zeolite comprises a band at approximately 280 nm, wherein a ratio of an integral, peak-fitted ultraviolet-visible absorbance signal measured in arbitrary units (a.u.) for the band at approximately 280 nm to an integral peak-fitted ultraviolet-visible absorbance signal measured in arbitrary units (a.u.) for a band at approximately 340 nm is >about 2. The present invention further provides a method of making an metal-loaded aluminosilicate zeolite having a maximum pore opening defined by eight tetrahedral atoms from pre-existing aluminosilicate zeolite crystallites, wherein the metal is present in a range of from 0.5 to 5.0 wt. % based on the total weight of the metal-loaded aluminosilicate zeolite.

First claim

The invention claimed is:

1. An iron-loaded aluminosilicate zeolite-derived material having a maximum pore opening defined by eight tetrahedral atoms and having the framework type CHA, AEI, AFX, ERI, or LTA, obtained by a method comprising the steps of:
(i) introducing mesoporosity into aluminosilicate zeolite crystallites by application of an aqueous alkali treatment to dissolve silica or application of an aqueous acidic treatment to dissolve alumina in the aluminosilicate zeolite crystallites;
(ii) introducing the iron into the product of step (i) by wet impregnation or wet ion- exchange by contacting the product of step (i) with a mixture of an iron-containing reagent and a structure directing agent for the aluminosilicate zeolite; and
(iii) closing the mesopores of the product of step (ii), thereby producing the iron-loaded aluminosilicate zeolite-derived material, wherein an ultraviolet-visible absorbance spectrum of the iron-loaded aluminosilicate zeolite-derived material comprises a band at approximately 280 nm, and, wherein a ratio of an integral, peak-fitted ultraviolet-visible absorbance signal measured in arbitrary units (a.u.) for the band at approximately 280 nm to an integral, peak-fitted ultraviolet-visible absorbance signal measured in arbitrary units (a.u.) for a band at approximately 340 nm is greater than about 2.

2. The iron-loaded aluminosilicate zeolite-derived material according to claim 1 , wherein a ratio of an integral ultraviolet-visible absorbance signal measured in arbitrary units (a.u.) for the band at approximately 280 nm to an integral ultraviolet-visible absorbance signal measured in arbitrary units (a.u.) for a band at approximately 470 nm is >5.

3. The iron-loaded aluminosilicate zeolite-derived material according to claim 1 , wherein the iron is present in the range of from about 0.7 to about 3.0 wt. % based on the total weight of the iron-loaded aluminosilicate zeolite.

4. The iron-loaded aluminosilicate zeolite-derived material according to claim 1 , wherein a silicon-to-aluminium ratio of the aluminosilicate zeolite-derived material is from about 5 to about 15.

5. The iron-loaded aluminosilicate zeolite-derived material according to claim 1 having a Fe/Al atomic ratio of from about 0.032 to about 0.75.

6. The iron-loaded aluminosilicate zeolite-derived material according to claim 1 having a mesopore volume determined by nitrogen physisorption of >about 0.10 cm 3 /g and optionally a total pore volume of >about 0.30 cm 3 /g.

7. The iron-loaded aluminosilicate zeolite-derived material according to claim 1 comprising one or more than one of the transition elements selected from the group consisting of Ce, Cu, Mn, Pd and Pt.

8. A washcoat composition comprising an aqueous slurry of an iron-loaded aluminosilicate zeolite-derived material according to claim 1 .

9. A honeycomb monolith substrate comprising an iron-loaded aluminosilicate zeolite-derived material according to claim 1 , wherein the honeycomb monolith substrate is coated with a washcoat composition comprising an aqueous slurry of the iron-loaded aluminosilicate zeolite-derived material or the honeycomb monolith substrate comprises an extrusion of the iron-loaded aluminosilicate zeolite-derived material.

10. An exhaust system comprising an injector for injecting a nitrogenous reductant from a source of nitrogenous reductant into a flowing exhaust gas and a source of nitrogenous reductant, which injector is disposed upstream from a honeycomb monolith substrate according to claim 9 .

11. The exhaust system according to claim 10 comprising a honeycomb monolith substrate comprising an oxidation catalyst for oxidising nitrogen monoxide in an exhaust gas flowing in the system to nitrogen dioxide, which honeycomb monolith substrate comprising the oxidation catalyst is disposed upstream of the honeycomb monolith substrate comprising the iron-loaded aluminosilicate zeolite-derived material.

Assignees

• Johnson Matthey Catalysts Germany Gmbh
• Johnson Matthey Plc

Inventors

• Bauer Juergen
• Casci John Leonello
• Dotzel Ralf
• Muench Joerg
• Purova Ralitsa
• Schwieger Wilhelm
• Shahid Ameen
• Thangaraj Selvam
• Weissenberger Tobias

Classifications

• B01J2229/34

  Reaction with organic or organometallic compounds · CPC title

• B01J37/0018

  Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat) · CPC title

• B01J29/7607

  A-type · CPC title

• B01J29/7807

  A-type · CPC title

• F01N3/2842

  specially adapted for monolithic supports, e.g. of honeycomb type (F01N3/2853 - F01N3/2871 take precedence) · CPC title