IP Library Granted Patent US 9,260,318
Granted Patent B2
US 9,260,318 · App. 14/528,259 · Granted Feb 16, 2016

Mesoporous titanium dioxide nanoparticles and process for their production

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Quick Facts
Patent No.
US 9,260,318
App. No.
14/528,259
Granted
Feb 16, 2016
Kind
B2
Abstract

TiO 2 nanoparticles having improved consistent particle morphology, uniform particle size, and which contain uniform intra-particle pores in the mesopore size range are produced by wet chemical hydrolysis.

Claims (7)

1. A method for producing generally uniform TiO 2 nanoparticles of from 20 nm to 100 nm in size wherein each particle contains generally uniform pores in the mesopore size range having a generally narrow pore size distribution centered at a value between about 2 nm to about 12 nm comprising:

(i) forming an aqueous solution of a water soluble compound of titanium at a concentration of from 0.5 to 1.5 moles per liter in the presence of an alpha hydroxyl carboxylic acid at an acid to titanium molar ratio of from 0.02 to 0.2;

(ii) heating the aqueous solution to a temperature in the range of from 70° C. to 80° C. and maintaining that temperature for a period of from 1 hour to 3 hours, and then heating the aqueous solution to a temperature in the range of from 100° C. up to the refluxing temperature and maintaining that temperature for an additional period of from 2 hours to 4 hours;

(iii) cooling the solution to room or ambient temperature, and separating the reaction product.

2. The method of claim 1 wherein the reaction product is separated by (i) filtering; (ii) washing the separated reaction product to remove salts generated during the reaction sequence; and (iii) finishing the product by drying whereby water and organic contents are removed.

3. Method of claim 2 wherein finishing is achieved by heating the product at an elevated temperature in the range of from 200° C. to 500° C. under a flow of air.

4. The method of claim 1 , claim 2 or claim 3 wherein heating the aqueous solution to a temperature in the range of from 70° C. to 80° C. and maintaining that temperature for a period of from 1 hour to 3 hours according to step (ii) is conducted concurrently with adding anatase TiO 2 seeds to the aqueous solution at a seed to TiO 2 molar ratio of from 0.0005 to 0.0015.

Assignments (2)
SECURITY INTEREST Recorded Sep 26, 2025
From: TRONOX LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 072942/0255 →
RELEASE OF SECURITY INTEREST Recorded Apr 7, 2022
From: WILMINGTON TRUST, NATIONAL ASSOCIATION
To: TRONOX LLC
Reel/Frame 059629/0581 →