Process for continuously synthesizing zeolite crystals

Patent metadata

Field	Value
Publication number	US-11040884-B2
Application number	US-201816493172-A
Country	US
Kind code	B2
Filing date	Mar 12, 2018
Priority date	Mar 17, 2017
Publication date	Jun 22, 2021
Grant date	Jun 22, 2021

Abstract

The present invention relates to a process for preparing zeolite crystals continuously, comprising the continuous introduction of a composition capable of generating zeolite crystals into at least one crystallization reaction zone subjected to stirring means, giving said composition a flow characterized by a relative Reynolds number Rer of between 40 and 50 000, and the continuous recovery of the crystals formed according to a flow characterized by a net Reynolds number Ren of between 1 and 1500.

First claim

The invention claimed is:

1. Process for preparing zeolite crystals continuously, comprising at least the following steps:
a) continuous supply of a composition capable of generating zeolite crystals;
b) continuous introduction of said composition into at least one crystallization reaction zone subjected to stirring means, giving said composition a flow characterized by a relative Reynolds number Re r of between 40 and 50 000, limits included,
c) continuous recovery of the crystals formed in step b) according to a flow characterized by a net Reynolds number Re n of between 1 and 1500, limits included.

2. Process according to claim 1 , wherein the difference between the relative Reynolds number Re r and the net Reynolds number Re n is greater than 50.

3. Process according to claim 1 , for preparing crystals of a zeolite of MFI type, a zeolite of MOR type, of OFF type, of MAZ type, of CHA type and of HEU type, a zeolite of FAU type, a zeolite of EMT type or a zeolite of LTA type.

4. Process according to claim 3 , for preparing zeolite crystals, where the zeolite is chosen from zeolites of MFI type, of FAU type, of LTA type, the zeolites of CHA type and the zeolites of HEU type.

5. Process according to claim 1 , comprising at least the following steps:
1) continuous preparation of a composition capable of generating zeolite crystals, in order to obtain a synthesis medium,
2) addition of seed to the synthesis medium obtained in step 1),
3) continuous operation, under stirring, of the reaction for forming zeolite crystals, according to steps a), b) and c) according to claim 1 ,
4) continuous filtration in order to separate the crystals obtained from the mother liquors, and
5) optionally recycling of the mother liquors.

6. Process according to claim 1 , wherein the crystallization step is carried out at a temperature of between 60° C. and 200° C.

7. Process according to claim 1 , further comprising the addition, in one or more stages, before, after or during the crystallization step, of one or more seeding agents.

8. Process according to claim 7 , wherein the seeding agent is chosen from a nucleating gel, a crystal, a mineral particle and mixtures thereof.

9. Process according to claim 1 , which process is carried out in a tubular reactor.

10. Process according to claim 1 , carried out in a tubular reactor provided with internal systems of restrictions and with a pulsating device, and operated under particular conditions, namely:
an oscillation amplitude of the pulsating device of between 20 mm and 400 mm, and
an oscillation frequency of between 0.1 Hz and 2 Hz.

Assignees

• Arkema France

Inventors

• Nicolas Serge
• Lutz Cécile
• Dubois Jean-Luc
• Lecomte Yvan

Classifications

• C01B39/46

  Other types characterised by their X-ray diffraction pattern and their defined composition {(C01B39/023, C01B39/026, C01B39/06 take precedence)} · CPC title

• C01B39/14

  Type A · CPC title

• C01B39/02 Primary

  Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof · CPC title

• C01B39/023 Primary

  Preparation of physical mixtures or intergrowth products of zeolites chosen from group C01B39/04 or two or more of groups C01B39/14 - C01B39/48 · CPC title

• C01B39/20

  Faujasite type, e.g. type X or Y · CPC title