IP Library Granted Patent US 11,046,587
Granted Patent B2
US 11,046,587 · App. 16/308,928 · Granted Jun 29, 2021

Process for a continuous synthesis of zeolitic materials

Inventors: Stefan Marx (Ludwigshafen, DE); Stefanie Clade (Ludwigshafen, DE); Lena Arnold (Brasschaat, BE); Uwe Diehlmann (Hassloch, DE); Ulrich Mueller (Ludwigshafen, DE)
Assignee: BASF SE
C01B39/48B01D53/9418B01J19/0013B01J19/1812B01J29/06B01J29/061B01J29/072B01J29/7015B01J29/763C01B39/02C01B39/04B01J29/86B01J29/87B01J37/0045B01J37/32B01J2219/00033B01J2219/00099B01J2219/00162B01J2219/00164B01J2229/186B01J2229/36B01J2229/42C01P2002/72
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Quick Facts
Patent No.
US 11,046,587
App. No.
16/308,928
Granted
Jun 29, 2021
Kind
B2
Abstract

A continuous process for preparing a zeolitic material comprising (i) preparing a mixture comprising a source of YO 2 , optionally a source of X 2 O 3 , and a liquid solvent system; (ii) continuously feeding the mixture prepared in (i) into a continuous flow reactor at a liquid hourly space velocity in the range of from 0.3 to 20 h − 1 for a duration of at least 1 h; and (iii) crystallizing the zeolitic material from the mixture in the continuous flow reactor, wherein the mixture is heated to a temperature in the range of from 100 to 300° C.; wherein the volume of the continuous flow reactor is in the range of from 150 cm 3 to 75 m 3 , as well as to zeolitic materials which may be obtained according to the inventive process and to their use.

Claims (34)

1. A continuous process for preparing a zeolitic material, the process comprising:

continuously feeding a mixture comprising a source of YO 2 , optionally a source of X 2 O 3 , and a liquid solvent system, into a continuous flow reactor at a liquid hourly space velocity in the range of from 0.3 to 20 h −1 for a duration of at least 1 h; and

crystallizing the zeolitic material from the mixture in the continuous flow reactor, the crystallizing comprising heating the mixture to a temperature in a range of from 100 to 300° C. in the continuous flow reactor,

wherein a volume of the continuous flow reactor is in the range of from 150 cm 3 to 75 m 3 .

2. The process of claim 1 , wherein the continuous flow reactor is a tubular reactor, a ring reactor, or a continuously oscillating reactor.

3. The process of claim 1 , wherein a wall of the continuous flow reactor comprises a metallic material.

4. The process of claim 1 , wherein a surface of the inner wall of the continuous flow reactor is lined with an organic polymer material.

5. The process of claim 1 , wherein, in the crystallizing, the mixture is heated under autogenous pressure.

6. The process of claim 1 , wherein the continuous flow reactor consists of a single stage.

7. The process of claim 1 , wherein no matter is added and/or removed from the reaction mixture during its passage through the continuous flow reactor in the crystallizing.

8. The process of claim 1 , further comprising:

preheating the mixture while feeding the mixture directly into the continuous flow reactor in the continuously feeding.

9. The process of claim 1 , further comprising:

quenching the reaction product effluent continuously exiting the reactor in the crystallizing with a liquid comprising a solvent and/or via expansion of the reaction product effluent;

and/or,

isolating the zeolitic material obtained in the crystallizing or quenching;

and/or,

washing the zeolitic material obtained in the crystallizing, quenching, or isolating;

and/or,

drying the zeolitic material obtained in the crystallizing, quenching, isolating, or washing;

and/or,

calcining the zeolitic material obtained in the crystallizing, quenching, isolating, washing, or drying.

10. The process of claim 9 , wherein the isolating is performed, and

wherein a supernatant obtained from the isolating of the zeolitic material, and/or

wherein a feed having the same composition as the supernatant, is not at any point recycled to the reaction mixture during its passage through the continuous flow reactor.

11. The process of claim 1 , wherein Y comprises Si, Sn, Ti, Zr, and/or Ge.

12. The process of claim 1 , wherein X comprises Al, B, In, and/or Ga.

13. The process of claim 1 , wherein the mixture comprises substantially no phosphorous and/or phosphorous comprising compounds.

14. A zeolitic material, obtained by the process of claim 1 .

15. A process, comprising employing the zeolitic material of claim 14 as a molecular sieve, as an adsorbent, for ion-exchange, as a catalyst, and/or as a catalyst support.

16. The process of claim 1 , wherein the volume of the continuous flow reactor is in the range of from 175 cm 3 to 1 m 3 .

17. The process of claim 1 , wherein the volume of the continuous flow reactor is at least 200 cm 3 .

18. The process of claim 1 , wherein the liquid hourly space velocity is no more than 8 h −1 .

19. The process of claim 1 , wherein the liquid hourly space velocity is in a range of from 4 to 6 h −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 11, 2018
From: MARX, STEFAN; CLADE, STEFANIE; ARNOLD, LENA; DIEHLMANN, UWE; MUELLER, ULRICH
To: BASF SE
Reel/Frame 047741/0520 →
Priority Claims (1)
EP 16174896 · Jun 17, 2016 · regional
Continuity (1)
Related Publication 20190144290A1 · May 16, 2019