Process for preparing a zeolitic material having a framework type fer

Patent metadata

Field	Value
Publication number	US-2021198114-A1
Application number	US-201917058338-A
Country	US
Kind code	A1
Filing date	Jul 26, 2019
Priority date	Jul 27, 2018
Publication date	Jul 1, 2021
Grant date	—

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.

First claim

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 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 preferably 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 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, 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.

Assignees

• Basf Se

Inventors

• Parvulescu Andrei-Nicolae
• Mcguire Robert
• Mueller Ulrich
• Kromer Alexander

Classifications

• C01B39/04 Primary

  using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound · CPC title

• B01J29/65

  of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38, as exemplified by patent documents US4046859, US4016245 and US4046859, respectively · CPC title

• C01B39/445 Primary

  using at least one organic template directing agent · CPC title

• F01N3/2066

  Selective catalytic reduction [SCR] · CPC title

• F01N2570/14

  Nitrogen oxides · CPC title