Porous iron-silicate with radially developed branch, and iron-carbide/silica composite catalyst prepared therefrom

Patent metadata

Field	Value
Publication number	US-10081008-B2
Application number	US-201515122332-A
Country	US
Kind code	B2
Filing date	May 15, 2015
Priority date	May 16, 2014
Publication date	Sep 25, 2018
Grant date	Sep 25, 2018

Abstract

The present invention provides an iron-carbide/silica composite catalyst that is highly reactive to a Fischer-Tropsch synthesis by firstly forming an iron-silicate structure having large specific surface area and well-developed pores through a hydrothermal reaction of an iron salt with a silica particle having a nanostructure, and then activating the iron-silicate structure in a high temperature carbon monoxide atmosphere. When using the iron-carbide/silica composite catalyst according to the present invention in the Fischer-Tropsch synthesis reaction, it is possible to effectively prepare liquid hydrocarbon with a high CO conversion rate and selectivity.

First claim

The invention claimed is:

1. A method of preparing a porous iron-silicate with radially developed branches, comprising the steps of:
(i) heating a silica solution wherein a silica particle is mixed with a basic reagent;
(ii) introducing an aqueous solution containing an iron salt hydrate to said heated silica solution; and
(iii) decomposing a mixed solution of the iron salt hydrate and silica through a high-temperature hydrothermal reaction to form the porous iron-silicate.

2. The method of claim 1 , wherein the silica particle has a surface area of 50˜1000 m 2 /g and a pore volume of 0.2˜3.0 cm 3 /g.

3. The method of claim 1 , wherein the basic reagent is sodium hydroxide and the amount of solid sodium hydroxide used is 0.5 to 2 times with respect to the weight of silica.

4. The method of claim 1 , wherein the silica particle is a silica nanobead, a silica sol, or a silica structure having mesopores.

5. The method of claim 1 , wherein the iron hydrate used in said Step (ii) is selected from the group consisting of iron (III) chloride hexahydrate, iron (II) chloride tetrahydrate, iron (Ill) nitrate nonahydrate, iron (III) sulfate hydrate, iron (II) perchlorate hydrate, and iron (II) sulfate hydrate.

6. The method of claim 1 , wherein the hydrothermal reaction in said Step (iii) is carried out in an oil bath of 100° C. or higher by refluxing the reactants for 1˜24 hours.

7. The method of claim 1 , wherein the porous iron-silicate obtained after said Step (iii) is centrifuged at a speed of 3,000˜10,000 rpm for 10˜100 minutes.

8. A method of preparing an iron-carbide/silica composite catalyst, comprising the steps of:
preparing a porous iron-silicate with radially developed branches, wherein the preparing comprises:
(i) heating a silica solution wherein a silica particle is mixed with a basic reagent;
(ii) introducing an aqueous solution containing an iron salt hydrate to said heated silica solution; and
(iii) decomposing a mixed solution of the iron salt hydrate and silica through a high-temperature hydrothermal reaction to form the porous iron-silicate; and

activating, through a high temperature calcination step, the porous iron-silicate with radially developed branch.

9. The method of claim 8 , wherein the iron-carbide/silica composite catalyst is obtained by activating the porous iron-silicate under a carbon monoxide-containing atmosphere.

10. The method of claim 8 , wherein the size of iron-carbide particle loaded on the silica shell is 10˜100 nm.

11. The method of claim 8 , wherein the activated iron-carbide/silica catalyst is immersed in an organic passivation solvent for preventing oxidation.

12. The method of claim 11 , wherein the organic passivation solvent is ethanol or mineral oil.

13. The method of claim 8 , wherein the calcination temperature is in the range of 350° C.˜400° C.

Assignees

• Korea Inst Energy Res

Inventors

• Park Ji Chan
• Chun Dong Hyun
• Jung Heon
• Lee Ho Tae
• Yang Jung Il
• Hong Sung Jun

Classifications

• B01J35/1042

  Operations & Transport · mapped topic

• B01J37/009

  Preparation by separation, e.g. by filtration, decantation, screening · CPC title

• B01J35/1047

  Operations & Transport · mapped topic

• B01J35/1038

  Operations & Transport · mapped topic

• B01J37/10 Primary

  in the presence of water, e.g. steam · CPC title