Core-shell particles with catalytic activity

Patent metadata

Field	Value
Publication number	US-9956545-B2
Application number	US-201615237233-A
Country	US
Kind code	B2
Filing date	Aug 15, 2016
Priority date	May 30, 2011
Publication date	May 1, 2018
Grant date	May 1, 2018

Abstract

The present invention pertains to novel core-shell particles comprising a core of iron oxide and a shell of cobalt oxide, characterized in that they are spherical with a number average diameter, as measured by TEM, of between 1 and 20 nm. This invention is also directed to their uses in the manufacture of a catalyst, and to the method for preparing these particles, by precipitating cobalt oxide onto magnetite or hematite particles which are themselves precipitated from Fe(III) and optionally Fe(II) salts.

First claim

The invention claimed is:

1. Core-shell particles obtained according to a method comprising:
(a) preparing an aqueous solution comprising a ferric salt, at a temperature of less than 50° C.;
(b) adding at least one base to said aqueous solution, so as to obtain a suspension of iron oxide particles having a pH value of from 10 to 14;
(c) washing the suspension;
(d) adding a strong acid to the washed suspension to peptize the washed suspension;
(e) reacting at least one base with said peptized suspension, until the pH reaches a value from 10 to 14, at a temperature of from 50 to 95° C.;
(f) adding a cobalt salt to the heated suspension in order to obtain spherical particles having a core of iron oxide and a shell comprising cobalt oxide, wherein the spherical particles comprise a core of iron oxide and a shell of Co 3 O 4 , characterized in that the core-shell particles are spherical with a number average diameter, as measured by TEM, of between 1 and 20 nm.

2. The core shell particles according to claim 1 , characterized in that the aqueous solution comprising the ferric salt further includes a ferrous salt in a molar ratio of Fe(III) to Fe(II) of 2:1, whereby the iron oxide particles are magnetite particles.

3. The core shell particles according to claim 1 , characterized in that the ferric salt is ferric nitrate, ferric chloride or ferric hydroxide.

4. The core shell particles according to claim 2 , characterized in that the ferrous salt is ferrous nitrate, ferrous chloride or ferrous hydroxide.

5. The core shell particles according to claim 1 characterized in that the cobalt salt is cobalt nitrate, cobalt chloride or cobalt sulphate.

6. The core shell particles according to claim 1 , characterized in that the strong acid is nitric acid or hydrochloric acid.

7. Core-shell particles according to claim 1 , characterized in that the core comprises magnetite or hematite and the shell comprises Co 3 O 4 .

Assignees

• Total Raffinage Chimie

Inventors

• Calderone Vincenzo Roberto
• Shiju Nirappurackal Raveendran
• Rothenberg Gad
• Curulla-Ferre Daniel

Classifications

• B01J23/75 Primary

  Cobalt · CPC title

• B01J37/32

  Freeze drying, i.e. lyophilisation · CPC title

• B01J35/008

  Operations & Transport · mapped topic

• B01J37/0072

  Preparation of particles, e.g. dispersion of droplets in an oil bath · CPC title

• B01J37/0221

  of particles · CPC title