IP Library Granted Patent US 10,875,012
Granted Patent B2
US 10,875,012 · App. 16/316,684 · Granted Dec 29, 2020

Process for the preparation of molybdenum disulfide nanoparticles supported on titania

Inventors: Robin Kolvenbach (Garching, DE); Marcello Stefano Rigutto (Amsterdam, NL); Thomas Weber (Amsterdam, NL); Lennart Van Haandel (Amsterdam, NL)
Assignee: Shell Oil Company
B01J27/051B01J21/063B01J27/0515B01J35/0013B01J35/1019B01J37/033B01J37/035B01J37/16C07C1/322C10G45/08B01J2523/00C07C2521/06C07C2527/051C07C2601/16C10G2300/202
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Quick Facts
Patent No.
US 10,875,012
App. No.
16/316,684
Granted
Dec 29, 2020
Kind
B2
Abstract

The invention relates to a process for the preparation of nanoparticles of MoS 2 supported on TiO 2 wherein the preparation is performed by reductive coprecipitation using aqueous solutions containing Ti and Mo precursor salts, and wherein MoS 2 may be non-promoted or Co-promoted. Further, the invention relates to the use of said nanoparticles as hydrodesulfurization catalysts.

Claims (17)

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.

Assignments (1)
CHANGE OF NAME Recorded Mar 7, 2022
From: SHELL OIL COMPANY
To: SHELL USA, INC.
Reel/Frame 059694/0819 →
Continuity (1)
Related Publication 20190151830A1 · May 23, 2019