IP Library Granted Patent US 11,554,964
Granted Patent B2
US 11,554,964 · App. 17/058,338 · Granted Jan 17, 2023

Process for preparing a zeolitic material having a framework type FER

Inventors: Andrei-Nicolae Parvulescu (Ludwigshafen, DE); Robert McGuire (Florham Park, NJ); Ulrich Mueller (Ludwigshafen, DE); Alexander Kromer (Ludwigshafen, DE)
Assignee: BASF SE
C01B39/445C01B39/04F01N3/2066C01P2006/14F01N2250/12F01N2570/14
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Quick Facts
Patent No.
US 11,554,964
App. No.
17/058,338
Granted
Jan 17, 2023
Kind
B2
Abstract

The present invention relates to a process for preparing a zeolitic material having a framework type FER and having a framework structure comprising silicon, aluminum, and oxygen, said process comprising (i) preparing an aqueous synthesis mixture comprising water; a zeolitic material having a framework type other than FER and having a framework structure comprising silicon, aluminum, and oxygen; a source of silicon other than the zeolitic material having a framework type other than FER; an organic structure directing agent comprising piperidine; a source of an alkali metal; and a source of a base; (ii) subjecting the aqueous synthesis mixture prepared according to (i) to hydrothermal synthesis conditions comprising heating the synthesis mixture to a temperature in the range of from 140 to 190° C. and keeping the synthesis mixture at a temperature in this range under autogenous pressure, obtaining a mother liquor comprising a solid material which comprises the zeolitic material having a framework type FER.

Claims (43)

1. A process for preparing a zeolitic material having a framework type FER and having a framework structure comprising silicon, aluminum, and oxygen, the process comprising:

preparing an aqueous synthesis mixture comprising water; a zeolitic material having a framework type other than FER and having a framework structure comprising silicon, aluminum, and oxygen; a source of silicon other than the zeolitic material having a framework type other than FER; an organic structure directing agent comprising piperidine; a source of an alkali metal; and a source of a base;

subjecting the aqueous synthesis mixture to hydrothermal synthesis conditions comprising heating the aqueous synthesis mixture to a temperature in the range of from 140 to 190° C. and keeping the synthesis mixture at a temperature in this range under autogenous pressure, obtaining a mother liquor comprising a solid material which comprises the zeolitic material having a framework type FER.

2. The process of claim 1 , wherein in in the framework structure of the zeolitic material having a framework type other than FER, the molar ratio of silicon relative to aluminum, calculated as SiO 2 :Al 2 O 3 , is in the range of from 2:1 to 40:1.

3. The process of claim 1 , wherein the framework type of the zeolitic material having a framework type other than FER is at least one selected from the group consisting of FAU, CHA, LEV, and AEI.

4. The process of claim 1 , wherein the framework type of the zeolitic material having a framework type other than FER is CHA,

wherein in the framework structure of the zeolitic material having a framework type other than FER, the molar ratio of silicon relative to aluminum, calculated as SiO 2 :Al 2 O 3 , is in the range of from 5:1 to 30:1.

5. The process of claim 1 , wherein the framework type of the zeolitic material having a framework type other than FER is FAU,

wherein in the framework structure of the zeolitic material having a framework type other than FER, the molar ratio of silicon relative to aluminum, calculated as SiO 2 :Al 2 O 3 , is in the range of from 2:1 to 8:1.

6. The process of claim 1 , wherein the framework type of the zeolitic material having a framework type other than FER is AEI,

wherein in the framework structure of the zeolitic material having a framework type other than FER, the molar ratio of silicon relative to aluminum, calculated as SiO 2 :Al 2 O 3 , is in the range of from 2:1 to 30:1.

7. The process of claim 1 , wherein the framework type of the zeolitic material having a framework type other than FER is LEV,

wherein in the framework structure of the zeolitic material having a framework type other than FER, the molar ratio of silicon relative to aluminum, calculated as SiO 2 :Al 2 O 3 , is in the range of from 2:1 to 30:1.

8. The process of claim 1 , wherein the organic structure directing agent comprises from 95 to 100 weight-% piperidine and from 0 to 1 weight % hexamethylene imine, each relative to the weight of the organic structure directing agent.

9. The process of claim 1 , wherein the source of silicon other than the zeolitic material having a framework type other than FER comprises at least one selected from the group consisting of a silicate, a silica gel, a silica sol, a silica powder, a solid silica gel, and a colloidal silica.

10. The process of claim 1 , wherein in the aqueous synthesis mixture, the weight ratio of the zeolitic material having a framework type other than FER relative to the source of a base is in the range of from 1:1 to 1:4.

11. The process of claim 1 , wherein the preparing the aqueous synthesis mixture comprises:

mixing water with the source of an alkali metal and the source of a base, obtaining a first mixture;

adding the source of silicon other than the zeolitic material having a framework type other than FER to the first mixture, obtaining a second mixture;

adding the zeolitic material having a framework type other than FER to the second mixture, obtaining a third mixture; and

adding the organic structure directing agent comprising piperidine to the third mixture, obtaining a fourth mixture;

or wherein the preparing the aqueous synthesis mixture according to (i) comprises:

mixing water with the source of an alkali metal and the source of a base, obtaining a first mixture;

adding the organic structure directing agent comprising piperidine and the zeolitic material having a framework type other than FER to the first mixture, obtaining a second mixture; and

adding the source of silicon other than the zeolitic material having a framework type other than FER to the second mixture, obtaining a third mixture.

12. The process of claim 1 , further comprising:

optionally cooling the mother liquor to a temperature in the range of from 10 to 50° C.; and

separating the solid material from the mother liquor.

13. The process of claim 12 , further comprising:

calcining the solid material

in a gas atmosphere having a temperature in the range of from 450 to 650° C.

14. The process of claim 12 , further comprising

subjecting the solid material to ion-exchange conditions.

15. The process of claim 14 , wherein the subjecting the solid material to ion-exchange conditions comprises

bringing a solution comprising ammonium ions in contact with the solid material, obtaining a solid material in its ammonium form;

optionally drying the solid material in its ammonium form in a gas atmosphere;

optionally calcining the solid material in its ammonium form in a gas atmosphere, obtaining the H-form of the solid material; and

bringing a solution comprising ions of one or more transition metals in contact with the solid material in its ammonium form or in contact with the H-form of the solid material.

16. A solid material comprising a zeolitic material having a framework type FER, or obtained by the process of claim 1 .

17. The solid material of claim 16 , having a molar ratio of silicon relative to aluminum, calculated as SiO 2 :Al 2 O 3 , in the range of from 2:1 to 150:1.

18. The solid material of claim 16 , having a micropore volume in the range of from 0.01 to 0.50 ml/g.

19. A method for catalytic reduction of nitrogen oxides in an exhaust gas stream of a diesel engine, comprising contacting the solid material of claim 16 with the exhaust gas stream.

20. A method for isomerization of olefins, comprising contacting the solid material of claim 16 with the olefins.

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 Nov 24, 2020
From: PARVULESCU, ANDREI-NICOLAE; MCGUIRE, ROBERT; MUELLER, ULRICH; KROMER, ALEXANDER
To: BASF SE
Reel/Frame 054458/0216 →
Priority Claims (1)
EP 18185968 · Jul 27, 2018 · regional
Continuity (1)
Related Publication 20210198114A1 · Jul 1, 2021