Iron-silicon oxide particles having an improved heating rate

Patent metadata

Field	Value
Publication number	US-10204723-B2
Application number	US-201314418989-A
Country	US
Kind code	B2
Filing date	Jul 17, 2013
Priority date	Aug 7, 2012
Publication date	Feb 12, 2019
Grant date	Feb 12, 2019

Abstract

Core-shell particles containing crystalline iron oxide in the core and amorphous silicon dioxide in the shell and in which
a) the shell contains from 5 to 40% by weight of silicon dioxide, b) the core contains
b1) from 60 to 95% by weight of iron oxide and b2) from 0.5 to 5% by weight of at least one doping component selected from the group consisting of aluminum, calcium, copper, magnesium, silver, titanium, yttrium, zinc, tin and zirconium,
c) where the % by weight indicated are based on the core-shell particles and the sum of a) and b) is at least 98% by weight of the core-shell particles, d) the core has lattice plane spacings of 0.20 nm, 0.25 nm and 0.29 nm, in each case+/−0.02 nm, determined by means of HR-TEM.

First claim

The invention claimed is:

1. Core-shell particles comprising crystalline iron oxide in the core and amorphous silicon dioxide in the shell, wherein
the shell consists of silicon dioxide and wherein silicon dioxide makes up from 5 to 40% by weight of the total weight of the core-shell particles,
the core consists of iron oxide and at least one doping component selected from the group consisting of aluminium, calcium, copper, magnesium, zinc and tin, wherein
iron oxide makes up from 60 to 95% by weight of the total weight of the core-shell particles and
the total amount of the at least one doping component make up from 0.5 to 5% by weight of the total weight of the core-shell particles,

wherein the total weight of the silicon dioxide, the iron oxide, and the at least one doping component equals 100% by weight,
the core has lattice plane spacings of 0.20 nm, 0.25 nm and 0.29 nm, in each case+/−0.02 nm, determined by means of high resolution transmission electron microscopy.

2. Core-shell particles according to claim 1 , wherein no lattice plane spacings which can be assigned to the doping component can be detected by X-ray diffraction or HR-TEM within a crystalline structure of the iron oxide.

3. Core-shell particles according to claim 1 , wherein the doping component is aluminium or zinc.

4. Core-shell particles according to claim 3 , wherein the proportion of doping component is from 1 to 2% by weight of the total weight of the core-shell particles.

5. Core-shell particles according to claim 1 , wherein the ratio of (magnetite+maghemite) to haematite determined by means of X-ray diffraction is from 70:30 to 95:5 and that of magnetite to maghemite is from 50:50 to 90:10.

6. Core-shell particles according to claim 1 , wherein a compound comprising the elements iron, silicon and oxygen and in the HR transmission electron micrograph have a spacing of the lattice planes of 0.31+/−0.01 nm and are present between the core and the shell.

7. Core-shell particles according to claim 1 , wherein the core-shell particles have been modified by adsorption, reaction on the surface or complexation of or with inorganic and organic reagents.

8. A process for producing the core-shell particles according to claim 1 , comprising:
igniting and reacting a mixture comprising
an aerosol obtained by atomization of a solution comprising in each case an oxidizable and/or hydrolysable iron compound, and in each case at least one dopant selected from the group consisting of aluminium, calcium, copper, magnesium, silver, titanium, zinc, tin and zirconium,
a hydrogen-containing fuel gas and
an oxygen-containing gas

in a first zone of a flow reactor;
adding a hydrolysable and/or oxidizable silicon compound to the reaction mixture in a second zone of the flow reactor; and then
optionally cooling the reaction mixture and separating the solid from materials in gaseous or vapour form; and then
optionally subsequently treating the solid with an agent for surface modification.

9. The process according to claim 8 , wherein in zone 1 the average residence time is from 10 ms to 1 ms and the temperature is from 800 to 1300° C. and in zone 2 the average residence time is from 0.1 to 10 s and the temperature is from 400 to 900° C.

10. The process according to claim 8 , wherein the silicon compound is at least one selected from the group consisting of SiCl 4 , CH 3 SiCl 3 , (CH 3 ) 2 SiCl 2 , (CH 3 ) 3 SiCl, HSiCl 3 , (CH 3 ) 2 HSiCl and CH 3 C 2 H 5 SiCl 2 , H 4 Si, Si(OC 2 H 5 ) 4 and Si(OCH 3 ) 4 .

11. The process according to claim 8 , wherein water or steam is additionally introduced in zone 2.

12. The process according claim 8 , wherein the agent for modifying the surface is an organosilane, a silazane or a polysiloxane.

13. Core-shell particles according to claim 1 , wherein the core-shell particles are suitable as constituent of rubber mixtures, as constituent of polymer preparations, as constituent of adhesive compositions, as constituent of shaped polymer composites which can be obtained by welding in an alternating electromagnetic field, and for producing dispersions and for the immobilization of enzymes.

Assignees

• Katusic Stipan
• Alff Harald
• Albers Peter
• Herzog Harald
• Kress Peter
• Evonik Degussa Gmbh

Inventors

• Katusic Stipan
• Alff Harald
• Albers Peter
• Herzog Harald
• Kress Peter

Classifications

• C01G49/00 Primary

  Compounds of iron · CPC title

• C09C1/24

  Oxides of iron · CPC title

• C01P2002/50

  Solid solutions · CPC title

• C01G49/02

  Oxides; Hydroxides {(C01G49/0018 takes precedence)} · CPC title

• B05D1/02

  performed by spraying · CPC title