Process for the preparation of molybdenum disulfide nanoparticles supported on titania

Patent metadata

Field	Value
Publication number	US-10875012-B2
Application number	US-201616316684-A
Country	US
Kind code	B2
Filing date	Jul 13, 2016
Priority date	Jul 13, 2016
Publication date	Dec 29, 2020
Grant date	Dec 29, 2020

Abstract

The invention relates to a process for the preparation of nanoparticles of MoS2 supported on TiO2 wherein the preparation is performed by reductive coprecipitation using aqueous solutions containing Ti and Mo precursor salts, and wherein MoS2 may be non-promoted or Co-promoted. Further, the invention relates to the use of said nanoparticles as hydrodesulfurization catalysts.

First claim

That which is claimed is:

1. A two-step hydrolysis process for the preparation of nanoparticles of MoS 2 supported on TiO 2 , wherein the two-step process comprises: preparing a dispersion of blue TiO 2-X support particles by adding a base to an aqueous solution of TiCl 3 and maintaining a resulting mixture under hydrolysis conditions for a time period; keeping said dispersion under an inert atmosphere, and introducing an aqueous solution of thiomolybdate to said dispersion to form said nanoparticles; and recovering said nanoparticles that are polycrystalline rutile and brooktie.

2. A two-step process as recited in claim 1 , wherein said nanoparticles have a specific surface area in the range of from 100 to 130 m 2 /g.

3. A two-step process as recited in claim 1 , wherein the value of X of the formula TiO 2-X is between 0 and 0.3.

4. A two-step process as recited in claim 1 , wherein said thiomolybdate is ammonium tetrathiomolybdate [(NH 4 ) 2 MoS 4 ].

5. A two-step process as recited in claim 1 , wherein said nanoparticles comprise polycrystalline rutile-brookite.

6. A two-step hydrolysis process as recited in claim 1 , wherein said base is sodium hydroxide.

7. A two-step thermolysis process as recited in claim 1 , wherein said aqueous solution of thiomolybdate comprises ammonium tetrathiomolybdate dissolved in citric acid solution and added ammonia.

8. A hydrodesulfurization process, comprising: passing a reaction feed over a hydrodesulfurization catalyst comprising nanoparticles produced by the two-step process of claim 1 .

9. A two-step thermolysis process for the preparation of nanoparticles of MoS 2 supported on TiO 2 , wherein said two-step process comprises:
preparing a dispersion of blue TiO 2-X support particles by maintaining an acidic aqueous solution of TiCl 3 under thermolysis conditions for a time period;
maintaining said dispersion under an inert atmosphere, and introducing an aqueous solution of thiomolybdate to said dispersion to form said nanoparticles; and
recovering said nanoparticles that are crystalline and comprises rutile polymorph.

10. A two-step process as recited in claim 9 , wherein said nanoparticles have a specific surface area in the range of from 100 to 130 m 2 /g.

11. A two-step process as recited in claim 9 , wherein the value of X of the formula TO 2-X is between 0 and 0.3.

12. A two-step process as recited in claim 9 , wherein said thiomolybdate is ammonium tetrathiomolybdate [(NH 4 ) 2 MoS 4 ].

13. A two-step thermolysis process as recited in claim 9 , wherein said acidic aqueous solution of TiCl 3 includes hydrochloric acid.

14. A two-step thermolysis process as recited in claim 9 , wherein said aqueous solution of thiomolybdate comprises ammonium tetrathiomolybdate dissolved in citric acid solution and added ammonia.

Assignees

• Shell Oil Co

Inventors

• Kolvenbach Robin
• Rigutto Marcello Stefano
• Weber Thomas
• Van Haandel Lennart

Classifications

• B01J37/033

  Using Hydrolysis · CPC title

• B01J37/03

  Precipitation; Co-precipitation · CPC title

• B01J35/45

  Nanoparticles · CPC title

• B01J35/40

  characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77) · CPC title

• B01J27/0515

  with iron group metals or platinum group metals · CPC title