IP Library Granted Patent US 8,715,618
Granted Patent B2
US 8,715,618 · App. 12/994,058 · Granted May 6, 2014

Process for the direct synthesis of Cu containing zeolites having CHA structure

Inventors: Natalia Trukhan (Ludwigshafen, DE); Ulrich Mueller (Neustadt, DE); Ivor Bull (Ludwigshafen, DE)
Assignee: BASF SE
C01B39/48B01J29/763B01J29/7065
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Quick Facts
Patent No.
US 8,715,618
App. No.
12/994,058
Granted
May 6, 2014
Kind
B2
Abstract

A process for the preparation of a copper containing zeolitic material having CHA framework structure and a composition comprising the molar ratio (n YO2):X203 wherein X is a trivalent element, preferably Al, Y is a tetravalent element, preferably Si, and wherein n is preferably at least 20. The process comprising the preparation of an phosphor-free aqueous solution containing at least one source for X203 and at least one source for YO2, at least one structure directing agent suitable for the preparation of a zeolitic material having CHA framework structure, and at least one Cu source, and the process further comprising the hydrothermal crystallization of said aqueous solution obtaining a suspension containing the copper containing zeolitic material having CHA framework structure.

Claims (35)

1. A process for preparing a copper-containing zeolitic material having a CHA framework structure, the process comprising:

(i) preparing an aqueous solution comprising

at least one source for X 2 O 3 ,

at least one source for YO 2 ,

at least one structure directing agent suitable for preparing a zeolitic material having a CHA framework structure, and

at least one Cu source,

wherein said aqueous solution does not comprise a phosphor source and has an alkali metal content of 1000 ppm or less; and

(ii) hydrothermally crystallizing the aqueous solution of the preparing (i) which does not comprise a phosphor source, to obtain a suspension comprising the copper-containing zeolitic material having a CHA framework structure;

wherein the structure directing agent is

a mixture of 1-adamantyltrimethyl-ammonium hydroxide and benzyltrimethylammonium hydroxide, or

a mixture of 1-adamantyltrimethylammonium hydroxide and tetramethylammonium hydroxide, or

a mixture of 1-adamantyltrimethylammonium hydroxide and tetramethylammonium hydroxide, or

a mixture of 1-adamantyltrimethylammonium hydroxide and benzyltrimethylammonium hydroxide and tetramethylammonium hydroxide,

wherein a molar ratio of 1-adamantyltrimethylammonium hydroxide to benzyltrimethylammonium hydroxide or to tetramethylammonium hydroxide, or to a sum of benzyltrimethylammonium hydroxide and tetramethylammonium hydroxide, is in a range of from 1:5 to 1:1, and

wherein the copper-containing zeolitic material has a composition comprising a molar ratio

( n YO 2 ):X 2 O 3

wherein X is a trivalent element, Y is a tetravalent element, and n is at least 10.

2. The process of claim 1 , wherein X is at least one selected from the group consisting of AI, B, In, and Ga, and wherein Y is at least one selected from the group consisting of Si, Sn, Ti, Zr, and Ge.

3. The process of claim 2 , wherein X is Al and Y is Si.

4. The process of claim 1 , wherein an aqueous solution comprising Cu and ammonia is employed as a Cu source.

5. The process of claim 1 , wherein, for the preparing (i), the at least one source for YO Z , the at least one source for X Z 0 3 , and the at least one Cu source are employed in such amounts that the aqueous solution obtained according to (i) exhibits a molar ratio

( n YO 2 ):X 2 O 3

wherein n is at least 10,

and a molar ratio

( m Cu):(( n YO 2 )+X 2 O 3 )

wherein m is at least 0.005.

6. The process of claim 1 , wherein the pH of the aqueous solution subjected to the hydrothermally crystallizing (ii) is in a range of from 12 to 14.

7. The process of claim 1 , wherein the hydrothermally crystallizing (ii) is carried out at a temperature in a range of from 100 to 200° C. and for a time period of from 12 to 144 h.

8. The process of claim 1 , wherein the aqueous solution subjected to the hydrothermally crystallizing (ii) comprises a La source.

9. The process of claim 1 , further comprising

(iii) separating the copper-containing zeolitic material from the suspension obtained in the hydrothermally crystallizing (ii);

(iv) drying the copper-containing zeolitic material, separated in (iii), at a temperature in a range of from 100 to 150° C.; and

(v) calcining the copper-containing zeolitic material, dried in (iv), at a temperature in a range of from 300 to 600° C.

10. The process of claim 1 , wherein, after the preparing (i), no Cu source is employed.

11. A copper-containing zeolitic material having framework structure CHA, obtained by the process of claim 1 .

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 Dec 1, 2010
From: TRUKHAN, NATALIA; MUELLER, ULRICH; BULL, IVOR
To: BASF SE
Reel/Frame 025405/0414 →
Priority Claims (1)
EP 08156625 · May 21, 2008 · regional
Continuity (1)
Related Publication 20110076229A1 · Mar 31, 2011