Process for manufacture of NOx storage materials

Patent metadata

Field	Value
Publication number	US-10449522-B2
Application number	US-201615747240-A
Country	US
Kind code	B2
Filing date	Jul 29, 2016
Priority date	Jul 30, 2015
Publication date	Oct 22, 2019
Grant date	Oct 22, 2019

Abstract

Processes for manufacturing nitrogen oxide storage materials and lean NOx trap catalysts are disclosed. Also disclosed are nitrogen oxide storage material made by processes comprising barium carbonate (BaCO 3 ) and ceria (CeO 2 ) by using Ba(OH) 2 instead of most or all Ba(OOCH 3 ) 2 to reduce cost and reduce harmful byproducts. Aspects of the present invention also relate generally to lean NO x trap (LNT) comprising nitrogen oxide storage materials.

First claim

The invention claimed is:

1. A process for manufacturing barium carbonate (BaCO 3 ) supported on ceria (CeO 2 ), the process comprising:
mixing Ba(OH) 2 with CeO 2 and H 2 O to provide a mixture;
drying the mixture at a temperature in the range of about 100° C. to about 150° C. to provide a dried mixture; and
calcining the dried mixture at a temperature in the range of about 40° C. to about 700° C.;
wherein the dried mixture is calcined in an air atmosphere at a temperature in the range of about 40° C. to about 450° C. or wherein the dried mixture is calcine in a CO 2 gas atmosphere at a temperature in the range of about 400° C. to about 700° C.

2. The process of claim 1 , wherein the dried mixture is calcined in an air atmosphere at a temperature in the range of about 40° C. to about 450° C.

3. The process of claim 1 , wherein the dried mixture is calcined in a CO 2 as atmosphere at a temperature in the range of about 400° to about 700° C.

4. The process of claim 3 , wherein the dried mixture is calcined for a period of time in the range of about 30 minutes to about 120 minutes.

5. The process of claim 4 , wherein the dried mixture is calcined for a period of time in the range of about 45 minutes to about 75 minutes.

6. The process of claim 4 , wherein the dried mixture is heated from room temperature to the calcining temperature over a period of about 150 minutes to about 210 minutes.

7. The process of claim 1 , wherein an amount of Ba(OH) 2 in the mixture of Ba(OH) 2 , CeO 2 , and H 2 O is in the range of 2% to about 15% by weight, and an amount of H 2 O in the mixture of Ba(OH) 2 , CeO 2 , and H 2 O is in the range of 30% to about 50% by weight.

8. The process of claim 1 , wherein an amount of Ba(OH) 2 in the mixture of Ba(OH) 2 , CeO 2 , and H 2 O is in the range of 10% to about 15% by weight, and an amount of H 2 O in the mixture of Ba(OH) 2 , CeO 2 , and H 2 O is in the range of 35% to about 45% by weight.

9. The process of claim 1 , wherein the mixture is dried at a temperature in the range of about 125° C. to about 135° C. for a period of time in the range of about 8 hours to about 18 hours.

10. The process of claim 1 , wherein the mixture is dried for a period of time in the range of about 10 hours to about 14 hours.

11. The process of claim 1 , wherein the mixture is milled in a ball mill for a period of time in the range of about 30 minutes to about 60 minutes.

12. A process for manufacturing a nitrogen oxide storage material, the process comprising:
preparing a mixture of Ba(OH) 2 , CeO 2 , and H 2 O, wherein Ba(OH) 2 is present in an amount up to the maximum solubility of Ba(OH) 2 in H 2 O at the temperature of the H 2 O, and CeO 2 is present in an amount of about 1.75 to about 2.0 times the amount of Ba(OH) 2 by weight;
milling the mixture for a period of time in the range of about 30 minutes to about 60 minutes to provide a milled mixture;
drying the milled mixture at a temperature in the range of about 110° C. to about 140° C. for a period of time in the range of about 8 hours to about 18 hours to provide a dried, milled mixture; and
calcining the dried, milled mixture at a temperature in the range of about 40° C. to about 700° C. for a period of time in the range of about 30 minutes to about 120 minutes.

13. The process of claim 12 , wherein the mixture is milled in a ball mill.

14. The process of claim 12 , wherein H 2 O is at a temperature in the range of about 10° C. to about 80° C. for preparing the mixture, and Ba(OH) 2 is present in an amount in the range of about 25 g/L H 2 O to about 1014 g/L H 2 O corresponding to the solubility at the temperature of the H 2 O.

15. The process of claim 12 , wherein the dried, milled mixture is calcined in a CO 2 gas atmosphere.

16. The process of claim 15 , wherein at least a portion of the CO 2 gas in the calcining atmosphere is provided by substituting about 3% to about 15% by weight of the Ba(OH) 2 with Ba(OOCH 3 ) 2 .

17. The process of claim 15 , wherein the dried, milled mixture is calcined in a CO 2 gas atmosphere at a temperature in the range of about 400° C. to about 700° C.

18. The process of claim 12 , wherein the dried, milled mixture is calcined at a temperature of about 650° C.

19. A process for manufacturing a nitrogen oxide storage material, the process comprising:
mixing Ba(OH) 2 with CeO 2 and H 2 O to provide a mixture, wherein the Ba(OH) 2 is present in an amount up to the maximum solubility of Ba(OH) 2 in H 2 O at the temperature of the H 2 O, and CeO 2 is present in an amount of about 1.75 to about 2.0 times the amount of Ba(OH) 2 by weight;
milling the mixture for a period of time in the range of about 30 minutes to about 60 minutes in a ball mill to provide a milled mixture;
drying the milled mixture at a temperature in the range of about 110° C. to about 140° C. for a period of time in the range of about 8 hours to about 18 hours to provide a dried, milled mixture; and
calcining the dried, milled mixture at a temperature in the range of about 200° C. to about 700° C. for a period of time in the range of about 60 minutes to about 120 minutes under a CO 2 gas atmosphere.

20. A nitrogen oxide storage material, produced by the process of claim 19 .

21. The nitrogen oxide storage material of claim 20 , having an average particle size in the range of about 2 microns to about 8 microns and a BET surface area of greater than 40 m 2 /g.

22. A lean NO x trap (LNT) catalyst, comprising the nitrogen oxide storage material of claim 20 .

23. The LNT catalyst of claim 22 , comprising a layer of LNT catalyst material on a honeycomb substrate.

Assignees

• Basf Corp

Inventors

• Hilgendorff Marcus
• Stohr Andreas
• Bidlingmaier Hermann
• Fellger Joachim

Classifications

• B01J37/0234

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