Process for the multi-reactor synthesis of zeolite crystals having a controlled particle size

Patent metadata

Field	Value
Publication number	US-11377361-B2
Application number	US-201816494613-A
Country	US
Kind code	B2
Filing date	Mar 12, 2018
Priority date	Mar 17, 2017
Publication date	Jul 5, 2022
Grant date	Jul 5, 2022

Abstract

The present invention relates to a process for preparing zeolite crystals having a multimodal particle size distribution, and the sizes of which are between 0.02 μm and 20 μm, said process comprising feeding at least two reactors each with a synthesis gel capable of forming zeolite crystals, carrying out a crystallization reaction, in parallel, in each of the at least two reactors, and mixing the reaction media of the at least two reactors, after the start of at least one of the crystallization reactions.

First claim

The invention claimed is:

1. Process for preparing zeolite crystals having a multimodal particle size distribution, where the particle sizes are between 0.02 μm and 20 μm, said process comprising at least the following steps:
a) preparing a synthesis gel by mixing at an applied shear rate of between 10,000 s −1 and 200,000 s −1 at least one source of silica, at least one source of alumina and optionally, at least one aqueous alkali or alkaline-earth metal hydroxide solution, where the synthesis gel contains between 0.005% and 10% by weight of seeding agent(s) relative to the synthesis gel,
b) feeding each of at least two reactors directly with the synthesis gel obtained in step a), where the synthesis gel is capable of forming zeolite crystals and is identical or different between the reactors,
c) carrying out a crystallization reaction, in parallel, in each of the at least two reactors, where the reactions are carried out simultaneously, sequentially or successively, to form zeolite crystals of different particle size distributions,
d) mixing the reaction media from the crystallization reactions of the at least two reactors at a time after start of the crystallization reaction, and
e) filtering the mixture of the reaction media obtained in step d), in order to separate the crystals produced from the mother liquors,
wherein one or more seeding agents are introduced into the synthesis gel(s) upstream of or inside at least one of the at least two reactors.

2. Process according to claim 1 , wherein the seeding agent is chosen from nucleating gels, zeolite crystals, mineral particles, and mixtures thereof.

3. Process according to claim 1 , wherein the reactors are selected from stirred reactors for syntheses in batch mode and tubular reactors for syntheses in continuous mode.

4. Process according to claim 3 , wherein 2, 3 or 4 of the reactors are tubular reactors.

5. Process according to claim 1 , wherein two or more of the reactors are either stirred reactors or tubular reactors.

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

7. Process according to claim 1 , wherein the crystallization reaction is carried out in the at least two reactors under a pressure between atmospheric pressure and 1.5 MPa.

8. Process according to claim 1 , wherein the reaction media of the at least two reactors operating in parallel are mixed at a time after start of the crystallization reaction but before the time in mixing step d).

9. Process according to claim 1 , wherein the mother liquors from the filtration step e) are recycled.

10. Process according to claim 1 , wherein the zeolite crystals are crystals of zeolite selected from the group consisting of zeolites of MFI type, zeolites of MOR type, zeolites of OFF type, zeolites of MAZ type, zeolites of CHA type, zeolites of HEU type, zeolites of FAU type, zeolites of EMT type and zeolites of LTA type.

Assignees

• Arkema France

Inventors

• Nicolas Serge
• Lutz Cécile

Classifications

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• B01J2219/00029

  Batch processes · CPC title

• B01J19/1812 Primary

  Tubular reactors · 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

• C01B39/26

  Mordenite type {(C01B39/023, C01B39/026, C01B39/06 take precedence)} · CPC title