IP Library Granted Patent US 11,872,543
Granted Patent B2
US 11,872,543 · App. 17/739,263 · Granted Jan 16, 2024

Hydrothermally stable methane oxidation catalyst

Inventors: Melanie M. Debusk (Oak Ridge, TN); Sreshtha Sinha Majumdar (Oak Ridge, TN); Josh A. Pihl (Oak Ridge, TN)
Assignee: UT-BATTELLE, LLC
B01J23/44B01J21/10B01J29/7015B01J35/04B01J35/1014B01J37/0207B01J37/08C01B39/48C01P2006/12C01P2006/16
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Quick Facts
Patent No.
US 11,872,543
App. No.
17/739,263
Granted
Jan 16, 2024
Kind
B2
Abstract

A method of manufacturing a methane oxidation catalyst and methane oxidation catalysts formed by the method are provided. The method includes providing a palladium (Pd)-based catalyst including Pd dispersed onto a support. A magnesium (Mg) precursor is introduced to the Pd-based catalyst by one of ion exchange or incipient wetness impregnation. After introducing the magnesium precursor to the Pd-based catalyst, the catalyst is dried and subjected to a final heat treatment that includes hydrothermal calcination. A method of methane oxidation in a lean exhaust environment via the methane oxidation catalyst is also provided.

Claims (23)

1. A method of manufacturing a methane oxidation catalyst, the method comprising:

providing a palladium (Pd)-based catalyst including Pd dispersed onto a support;

introducing a magnesium (Mg) precursor to the Pd-based catalyst by one of ion exchange or incipient wetness impregnation; and

after introducing the magnesium precursor to the Pd-based catalyst, drying the catalyst and subjecting the catalyst to a final heat treatment;

wherein the final heat treatment is hydrothermal calcination performed at a temperature in the range of 400 to 800° C. for a time period of 4 hours or more in the presence of water, oxygen, and nitrogen.

2. The method of claim 1 , wherein the step of providing a Pd-based catalyst includes introducing a Pd precursor to the support.

3. The method of claim 2 , wherein the Pd precursor is Pd(NO 3 ) 2 .2H 2 O.

4. The method of claim 2 , wherein the support is a small-pore zeolite having a SiO 2 :Al 2 O 3 ratio of 10:1 or greater.

5. The method of claim 2 , wherein the Pd precursor is introduced to the support by one of ion exchange or incipient wetness impregnation.

6. The method of claim 5 , wherein the Pd precursor is dispersed onto the support in an amount in the range of 1 to 5 wt. % based on the weight of the support.

7. The method of claim 5 , wherein the Pd precursor and Mg precursor are added sequentially, in that order.

8. The method of claim 1 , wherein the support is a high surface area Al 2 O 3 having a surface area greater than 90 m 2 /g.

9. The method of claim 1 , wherein the Mg precursor is Mg(NO 3 ) 2 .6H 2 O.

10. The method of claim 1 , wherein the molar ratio of Mg:Pd in the catalyst is in the range of 1:1 to 3:1.

11. The method of claim 1 , wherein the step of drying the catalyst is performed at a temperature in the range of 100 to 140° C. for a time period of between 2 and 5 hours.

12. A method of manufacturing a methane oxidation catalyst, the method comprising:

providing a palladium (Pd)-based catalyst including Pd dispersed onto a support;

introducing a magnesium (Mg) precursor to the Pd-based catalyst by one of ion exchange or incipient wetness impregnation; and

after introducing the magnesium precursor to the Pd-based catalyst, drying the catalyst and subjecting the catalyst to a final heat treatment;

wherein the step of providing a Pd-based catalyst includes introducing a Pd precursor to the support;

wherein the Pd precursor is introduced to the support by one of ion exchange or incipient wetness impregnation;

wherein the Pd precursor and Mg precursor are added sequentially, in that order;

wherein prior to the addition of the Mg precursor, the Pd-based catalyst is subjected to an intermediate heat treatment that is hydrothermal calcination performed at a temperature in the range of 400 to 800° C. for a time period of 4 hours or more in the presence of water, oxygen, and nitrogen.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jun 13, 2022
From: UT-BATTELLE, LLC
To: U. S. DEPARTMENT OF ENERGY
Reel/Frame 060176/0968 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 11, 2022
From: DEBUSK, MELANIE M.; SINHA MAJUMDAR, SRESHTHA; PIHL, JOSH A.
To: UT-BATTELLE, LLC
Reel/Frame 059892/0983 →
Continuity (2)
Provisional Application 63186965 · May 11, 2021
Related Publication 20220362747A1 · Nov 17, 2022