PROCESS FOR SYNTHESISING COATED ORGANIC OR INORGANIC PARTICLES

• US 20090186153A1
• Filed: 05/14/2007
• Published: 07/23/2009
• Est. Priority Date: 05/15/2006
• Status: Abandoned Application

• Current Assignee: Commissariat a L'Energie Atomique (AES Corporation), Centre National De La Recherche Scientifique, Ecole Nationale Supérieure de Chimie de Montpellier, Universite Montpellier II
• Original Assignee: Centre National De La Recherche Scientifique, Energies Alternatives Commissariat A L'Energie Atomique et AUX, Universite Montpellier II
• Inventors: Ruiz, Jean-Christophe, Hertz, Audrey, Sarrade, Stephane, Fournel, Bruno, Guizard, Christian, Julbe, Anne
• Application Number:
  US12/300,785
• Publication Number:
  US 20090186153A1
• Time in Patent Office: Days
• US Class Current: 427/216
• CPC Class Codes: B01J 13/02 Making microcapsules or microballoons for medical preparations A61K9/50
• CPC Class Codes: B01J 13/14 Polymerisation; cross-linking
• CPC Class Codes: B01J 19/26 Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
• CPC Class Codes: B01J 2219/00006 Large-scale industrial plants
• CPC Class Codes: B01J 2219/0004 Processes in series
• CPC Class Codes: B01J 2219/00768 vertical
• CPC Class Codes: B01J 3/008 Processes carried out under supercritical conditions

Abstract

A process for the “in situ” manufacture, in a pressurized CO₂ medium, of coated particles. The manufacturing process is characterized in that the steps of synthesising the particles and of coating these particles are coupled in such a way that the synthesised particles remain dispersed in a pressurized CO₂ medium at least until the coating. The device comprises a reactor for synthesising particles in a pressurized CO₂ medium; a means of injecting the coating material or precursor thereof into said reactor; a means of supplying said reactor with a pressurized CO₂ medium; in which the means of injecting the coating material or precursor thereof is coupled to the synthesis reactor in such a way that the injection of the coating material or precursor thereof into said reactor does not destroy the dispersion of the particles, in a pressurized CO₂ medium, in said reactor.

Claims

1. Process for manufacturing particles coated with a coating material, said process comprising the following steps:

(a) synthesising particles in a pressurized CO₂ medium,

(b) bringing the synthesised particles and the coating material or the precursors of said material into contact, in a pressurized CO₂ medium,

(c) coating the synthesised particles with the coating material, using the coating material directly, or after conversion of the precursors of the coating material into said coating material, and

(d) recovering the coated particles,

steps (a) and (b) being coupled such that the particles synthesised in step (a) remain dispersed in a pressurized CO₂ medium at least until step (c).

2. Process according to claim 1, in which the process is a batch, semi-continuous or continuous process.

3. Process according to claim 1, in which step (a) of synthesising the particles is followed by a step of sweeping the synthesised particles with pressurized CO₂ before carrying out step (b) of bringing said particles into contact with the coating material or precursors thereof.

4. Process according to claim 1, also comprising a step (x) of preparing the coating material before step (b) of bringing into contact.

5. Process according to claim 4, in which step (x) of preparing the coating material is either a synthesis of the coating material which uses a process chosen from a sol-gel process, a polymerization process, a prepolymerizaton process, a thermal decomposition process, or an organic or inorganic synthesis process;

or a solubilization of the coating material in a solvent or in a pressurized CO₂ medium.

6. Process according to claim 1, in which step (a) of synthesising the particles and step (b) of bringing said particles into contact with the coating material or precursors thereof are carried out in the same reactor.

7. Process according to claim 6, in which step (b) of bringing into contact consists in injecting the coating material or precursors thereof into said reactor containing the synthesised particles in a pressurized CO₂ medium.

8. Process according to claim 1, in which step (a) of synthesising the particles is carried out in a first reactor, the synthesised particles being transferred, in a pressurized CO₂ medium, into a second reactor, step (b) of bringing said synthesised particles into contact with the coating material or precursors thereof being carried out in said second reactor.

9. Process according to claim 8, in which the particles are transferred into the second reactor continuously or semi-continuously.

10. Process according to claim 8, in which step (h) of bringing into contact consists in injecting the coating material or precursors thereof into said second reactor containing, in a pressurized CO₂ medium, the synthesised particles.

11. Process according to claim 8, in which the coating material or precursors thereof is in a pressurized CO₂ medium when it is injected into said reactor.

12. Process according to claim 8, in which the coating material or precursors thereof is in an inorganic medium when it is injected into said reactor.

13. Process according to claim 8, in which step (b) of bringing said synthesised particles into contact with the coating material or precursors thereof is carried out in said second reactor, this second reactor being a nozzle comprising a first and a second injection inlet, and also an outlet;

in which the synthesised particles, in a pressurized CO₂ medium, are injected via the first inlet of the nozzle, and, at the same time as said particles, the coating material or precursors thereof is/are injected via the second inlet, in such a way that the bringing into contact of the synthesised particles with the coating material or precursors thereof is carried out in said nozzle; and

in which the coated particles or a mixture of particles and of coating material or precursors of said material is/are recovered via said outlet.

14. Process according to claim 8, in which step (b) of bringing said synthesised particles into contact with the coating material or precursors thereof is carried out in said second reactor, this second reactor being a tube reactor comprising a first end equipped with an inlet and a second end equipped with an outlet;

in which, on the one hand, in a pressurized CO₂ medium, the particles synthesised in the first reactor and, on the other hand, at the same time a said particles, the coating material or precursors thereof, are injected into said second reactor via the inlet in such a way that the bringing into contact of the synthesised particles with the coating material or precursors thereof is carried out in said second reactor; and

in which the coated particles or a mixture of particles and of coating material or precursors of said material is/are recovered via said outlet.

15. Process according to claim 13, in which step (c) of coating the particles is carried out in said second reactor, subsequent to bringing the particles, in a pressurized CO₂ medium, into contact with the coating material or precursors thereof.

16. Process according to claim 13, in which step (c) of coating the particles is carried out at the outlet of said second reactor.

17. Process according to claim 13, in which a mixture of particles and of coating material or precursors thereof is recovered at the outlet of said second reactor, the coating step (c) being carried out in a reactor for recovering this mixture, connected to the outlet of said nozzle.

18. Process according to claim 8, in which the coated particles are recovered in at least one recovery reactor connected to the outlet of said second reactor.

19. Process according to claim 18, in which the coated particles are recovered in at least two recovery reactors connected to the outlet of said second reactor, said recovery reactors being used alternately or successively.

20. Process according to claim 1, in which the coating of the particles in coating step (c) is carried out by means of a process of precipitating the coating material on said particles.

21. Process according to claim 20, in which the precipitation process is chosen from an antisolvent process, an atomization process in a supercritical medium and a phase separation process.

22. Process according to claim 1, in which the coating of the particles in coating step (c) is carried out by chemical conversion of said precursors into said coating material in the presence of the particles to be coated.

23. Process according to claim 22, in which the chemical conversion is chosen from a polymerization, the precursors of the coating material being a monomer and/or a prepolymer of the coating material;

a sol-gel synthesis;

a thermal decomposition process; and

an inorganic synthesis process.

24. Process according to claim 1, in which step (d) of recovering the coated particles comprises sweeping the coated particles with pressurized CO₂.

25. Process according to claim 1, in which step (d) of recovering the coated particles comprises expansion of the pressurized CO₂.

26. Process according to claim 1, in which the coated particles are recovered in a solvent or in a surfactant solution.

27. Process according to claim 1, in which the particles are chosen from metal particles;

particles of metal oxide(s);

ceramic particles;

particles of a catalyst or of a mixture of catalysts;

particles of a cosmetic product or of a mixture of cosmetic products; and

particles of a pharmaceutical product or of a mixture of pharmaceutical products.

28. Process according to claim 1, in which the particles are chosen from particles of titanium dioxide, of silica, of doped or undoped zirconium oxide, of doped or undoped ceria, of alumina, of doped or undoped lanthanum oxides, or of magnesium oxide.

29. Process according to claim 1, in which the coating material is a material chosen from a sintering agent, a friction agent, an anti-wear agent, a plasticizer, a dispersant, a crosslinking agent, a metallizing agent, a metallic binder, an anti-corrosion agent and an anti-abrasion agent.

30. Process according to claim 1, in which the coating material is chosen from an organic polymer, a sugar, a polysaccharide, a metal, a metal alloy and a metal oxide.

31. Process according to claim 1, in which the coating material is a polymer chosen from poly(methyl methacrylate) and polyethylene glycol;

a metal chosen from copper, palladium and platinum;

or a metal oxide chosen from magnesium oxide and alumina.

32. Process according to claim 31, in which, since the coating material is a polymer, its precursor is a monomer or a prepolymer of said polymer.

33. Process according to claim 1, in which the coated particles are chosen from yttrium-doped zirconium oxide particles coated with poly(methyl methacrylate), metal oxide catalyst particles coated with a noble metal, such as Ti oxide particles coated with Pd or Pt, and titanium dioxide particles coated with a polymer.

34. Process according to claim 1, in which the coated particles recovered constitute a nanophase powder of at least one oxide.

35. Process according to claim 1, in which the pressurized CO₂ medium is a supercritical CO₂ medium.