IP Library Granted Patent US 9,895,684
Granted Patent B2
US 9,895,684 · App. 14/534,642 · Granted Feb 20, 2018

Process for the preparation of zeolites having CHA structure

Inventors: Ivor Bull (Hopewell Junction, NY); Ulrich Müller (Neustadt, DE)
Assignee: BASF SE
B01J29/763B01D53/9418B01J29/7015B01J37/0246C01B39/00C01B39/02C01B39/04C01B39/46C01B39/48B01D2251/2067B01D2253/108B01D2255/20761B01D2255/50B01D2257/402B01D2257/404B01D2258/012B01J35/04Y02C20/10Y02P20/153
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Quick Facts
Patent No.
US 9,895,684
App. No.
14/534,642
Granted
Feb 20, 2018
Kind
B2
Abstract

Zeolites having CHA framework structure and a composition comprising the molar ratio (n SiO2): X203, wherein X is a trivalent element, and wherein n is at least 10, wherein the crystal size, as determined from Scanning Electron Microscopy, is greater than 1 micrometer and wherein the chabazite framework is phase-pure having an impurity of other zeolitic frameworks, such as RUT 25 as determined by X-ray Diffraction, of less than 5%. The process for the preparation comprises: (i) preparation of an aqueous solution containing at least one source for X203 , wherein X is selected from Al, B, Ga, and a mixture of two or more, and at least one source for SiO2, at least one organic structure directing agent (SDA) other than Tetramethylammonium hydroxide (TMAOH), acting as a template for the CHA structure, and Tetramethylammonium hydroxide (TMAOH), wherein the SDA or mixtures thereof are employed in such amounts that the aqueous solution in (i) exhibits a molar ratio of SDA : TMAOH of 0.01 to 5; (ii) hydrothermal crystallization of the aqueous solution according to (i); wherein the aqueous solution of (i) contains copper in an amount less than 0.005 Cu:((n YO2)+X203) where n is in the range of 10 to 50.

Claims (24)

1. A zeolitic material having framework structure CHA, having a composition comprising the molar ratio (n SiO 2 ):X 2 O 3 , wherein X is a trivalent element, and wherein X is selected from Al, B, Ga, and a mixture of two or more, and n is at least 10, obtainable by a process comprising:

(i) preparation of an aqueous solution containing:

at least one source for X 2 O 3 , wherein X is selected from Al, B, Ga, and a mixture of two or more,

at least one source for SiO 2 ,

at least one organic structure directing agent (SDA) other than Tetramethylammonium hydroxide (TMAOH) as a template for the CHA structure, and

Tetramethylammonium hydroxide (TMAOH),

wherein the SDA or mixtures thereof are employed in such amounts that the aqueous solution in (i) exhibits a molar ratio of SDA:TMAOH in the range of 0.01 to 5;

(ii) hydrothermal crystallization of the aqueous solution according to (i);

wherein the aqueous solution of (i) contains copper in an amount less than 0.005 Cu: ((n SiO 2 )+X 2 O 3 ) where n is at least 10, and

wherein the zeolitic material having framework structure CHA has a sodium content of 1000 ppm or less.

2. A method for the selective reduction (SCR) of nitrogen oxides NO x , for the oxidation of NH 3 or for the decomposition of N 2 O, the method comprising contacting a stream comprising NOx, NH 3 or N 2 O with a catalyst comprising the zeolitic material of claim 1 .

3. A method for catalyzing a chemical reaction, the method comprising using the zeolitic material of claim 1 as a catalytically active material in a chemical reaction.

4. A catalyst comprising the zeolitic material of claim claim 1 .

5. The zeolitic material of claim 1 , wherein the aqueous solution obtained in (i) and subjected to hydrothermal crystallization in (ii) is free of sodium.

6. The zeolitic material of claim 1 , wherein the aqueous solution obtained in (i) and subjected to hydrothermal crystallization in (ii) has a sodium content of 1000 ppm or less.

7. The zeolitic material of claim 1 , wherein the zeolitic material is free of sodium.

8. A zeolitic material having framework structure CHA, having a composition comprising the molar ratio (n SiO 2 ):X 2 O 3 , wherein X is a trivalent element, and wherein X is selected from Al, B, Ga, and a mixture of two or more, and n is at least 10, and wherein the crystal size of that zeolitic material, as determined from Scanning Electron Microscopy, is greater than 1 micrometer and wherein the chabazite framework is phase-pure having an impurity of other zeolitic frameworks of less than 5%, as determined by X-ray Diffraction, and

wherein the zeolitic material having framework structure CHA has a sodium content of 1000 ppm or less.

9. The zeolitic material of claim 8 , wherein the crystal size is in the range of greater than 1 micron to 5 microns.

10. The zeolitic material of claim 8 , wherein the chabazite framework is phase-pure having an impurity of other zeolitic frameworks of less than 1%.

11. A method for the selective reduction (SCR) of nitrogen oxides NO x , for the oxidation of NH 3 or for the decomposition of N 2 O, the method comprising contacting a stream comprising NOx, NH 3 or N 2 O with a catalyst comprising the zeolitic material of claim 8 .

12. A method for catalyzing a chemical reaction, the method comprising using the zeolitic material of claim 8 as a catalytically active material in a chemical reaction.

13. A catalyst comprising the zeolitic material of claim claim 8 .

14. The zeolitic material of claim 8 , wherein the zeolitic material is free of sodium.

Assignments (3)
NUNC PRO TUNC ASSIGNMENT Recorded Jan 24, 2025
From: BASF SE
To: BASF CATALYSTS LLC
Reel/Frame 070001/0877 →
NUNC PRO TUNC ASSIGNMENT Recorded Jan 24, 2025
From: BASF CATALYSTS LLC
To: BASF MOBILE EMISSIONS CATALYSTS LLC
Reel/Frame 070002/0453 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 9, 2016
From: BULL, IVOR; MÜLLER, ULRICH
To: BASF SE
Reel/Frame 037748/0156 →
Continuity (3)
Continuation 13511755
Provisional Application 61263831 · Nov 24, 2009
Related Publication 20150132215A1 · May 14, 2015