Fluidized bed reactor adapted for the production of biphased systems

Patent metadata

Field	Value
Publication number	US-11124871-B2
Application number	US-201616064067-A
Country	US
Kind code	B2
Filing date	Dec 16, 2016
Priority date	Dec 21, 2015
Publication date	Sep 21, 2021
Grant date	Sep 21, 2021

Abstract

A fluidized bed reactor designed for in situ gas phase impregnation. The reactor comprises a tube with an upstream zone and a downstream zone, the upstream zone and the downstream zone being separated by a separation filter. A method for a controlled-deposition of a sublimated precursor onto a fluidized solid support. The method is remarkable in that it is carried out in situ within the tube of the fluidized bed reactor in accordance with the fluidized bed reactor.

First claim

The invention claimed is:

1. A fluidized bed reactor, said fluidized bed reactor comprising:
a gas inlet and a gas outlet being located downstream from the gas inlet;
a tube made of quartz and inserted between the gas inlet and the gas outlet; and
a heating part connected to the tube,
wherein the tube comprises an upstream zone and a downstream zone, the upstream zone and the downstream zone being separated by a separation filter,
wherein the tube is inserted inside a first seal in the gas inlet and inside a second seal in the gas outlet; and
wherein at least one vibrator is connected to the tube, positioned outside the tube and distant from said tube, exclusively on a conduit between the gas inlet and the first seal.

2. The fluidized bed reactor according to claim 1 , wherein the tube is made of material which is resistant to temperature of at least up to 1,000° C. and is transparent.

3. The fluidized bed reactor according to claim 1 , wherein the upstream zone is delimited by the separation filter and by a first porous filter, and the downstream zone is delimited by the separation filter and by a second porous filter.

4. The fluidized bed reactor according to claim 3 , wherein the first porous filter is adjacent to the first seal and the second porous filter is adjacent to the second seal.

5. The fluidized bed reactor according to claim 1 , wherein the heating part is at least one of a heating cable, a heating jacket and a thermal activation source.

6. The fluidized bed reactor according to claim 1 , wherein the upstream zone of the tube is configured to be loaded of at least one precursor powder to be sublimated.

7. The fluidized bed reactor according to claim 1 , wherein the downstream zone of the tube is configured to be loaded with solid support.

8. The fluidized bed reactor according to claim 1 ,
wherein the upstream zone forms a cavity to be loaded with at least one solid precursor in powder form and the downstream zone forms a cavity to be loaded with a solid support in powder form; and
wherein the upstream zone is delimited by the separation filter and by a first porous filter, and the downstream zone is delimited by the separation filter and by a second porous filter, the second porous filter being structured and designed for containing inside the tube the solid support in powder form with particles of a size less than 20 μm.

9. The fluidized bed reactor according to claim 1 , wherein the upstream zone is delimited by the separation filter and by a first porous filter, and the downstream zone is delimited by the separation filter and by a second porous filter.

10. The fluidized bed reactor according to claim 1 , wherein the downstream zone of the tube is configured to be loaded with solid support.

11. A method for a controlled-deposition of particles onto a solid support, the method being carried out with a fluidized bed reactor and comprising the steps of:
(a) fluidization of at least one solid support in powder form; and
(b) impregnation of the fluidized solid support of step (a) by a sublimated precursor powder, wherein said fluidized bed reactor comprises:
a gas inlet and a gas outlet being located downstream from the gas inlet;
a tube made of quartz and inserted between the gas inlet and the gas outlet; and
a heating part connected to the tube, wherein the tube comprises an upstream zone and a downstream zone, the upstream zone and the downstream zone being separated by a separation filter,
wherein the tube is inserted inside a first seal in the gas inlet and inside a second seal in the gas outlet; and
wherein at least one vibrator is connected to the tube, positioned outside the tube and distant from said tube, exclusively on a conduit between the gas inlet and the first seal.

12. The method according to claim 11 , wherein the sublimated precursor powder is formed by heating a precursor powder to be sublimated.

13. The method according to claim 12 , wherein the precursor powder to be sublimated is an organometallic precursor comprising a metal derivative, the metal derivative being one of titanium, vanadium, iron, chromium, ruthenium, cobalt, iridium, nickel, copper, zinc, or manganese.

14. The method according to claim 12 , wherein the precursor powder to be sublimated is an organometallic precursor at least functionalized with an organic ligand.

15. The method according to claim 14 , wherein the method further comprises the step of removing the organic ligand, the step of removing the organic ligand being carried out by tuning the temperature.

16. The method according to claim 11 , wherein at least one of:
the solid support is a powder with a mean diameter size below 20 μm, and the solid support is made of particles.

17. The method according to claim 11 , wherein the step (a) is carried out with a flow of inert gas.

18. The method according to claim 11 , wherein step (b) is carried out at a temperature comprised between 150° C. and 190° C. under a flow of inert gas, the flow being comprised between 50 sccm and 1,000 sccm.

Assignees

• Luxembourg Inst Science & Tech List

Inventors

• Adjeroud Noureddine
• Arl Didier
• Lenoble Damien
• Sarr Mouhamadou Moustapha

Classifications

• C23C16/45555

  applied in non-semiconductor technology · CPC title

• B01J2208/00752

  Feeding · CPC title

• B01J2208/00212

  Plates; Jackets; Cylinders · CPC title

• B01J8/40

  with fluidised bed subjected to vibrations or pulsations · CPC title

• B01J2219/2423

  Separation means, e.g. membrane inside the reactor · CPC title