IP Library Granted Patent US 8,900,705
Granted Patent B2
US 8,900,705 · App. 13/297,869 · Granted Dec 2, 2014

Mesoporous titanium dioxide nanoparticles exhibiting bimodal pore size distributions and process for their production

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Quick Facts
Patent No.
US 8,900,705
App. No.
13/297,869
Granted
Dec 2, 2014
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 (11)

1. An oxide of titanium in the form of a powder comprising generally uniform nanoparticle spheres in 100 percent anatase crystalline phase, said spheres being from 20 nm to 100 nm in size and exhibiting bimodal pore size distributions wherein each spherical particle contains generally uniform pores in the mesopore size range which have a uniform pore size distribution centered at a value between about 2 nm to about 12 nm and the spheres exhibit an inter-particle pore size distribution centered at a value between about 15 nm and about 80 nm.

2. The oxide of titanium in the form of a powder comprising generally uniform nanoparticle spheres as claimed in claim 1 having a size in the range of 50 nm, intra-particle mesopores centered at about 6 nm and inter-particle mesopores centered at about 35 nm.

3. The oxide of titanium in the form of a powder comprising generally uniform nanoparticle spheres as claimed in claim 1 or claim 2 wherein the titanium has a crystallite size in the range of from about 4 nm to about 12 nm.

4. A titanium oxide product comprising a plurality of nanoparticle spheres as claimed in claim 1 , or claim 2 , having a pore volume in the range of from 0.2 to 0.6 cm 3 /g.

5. A titanium oxide product comprising nanoparticle spheres as claimed in claim 4 having bimodal pore size distributions centered at about 6 nm and about 35 nm, respectively, and having a pore volume in the range of about 0.6 cm 3 /g.

6. An oxide of titanium in the form of generally uniform nanoparticle spheres in 100 percent anatase crystalline phase having bimodal pore size distributions centered at 2 nm to 12 nm and 15 nm to 80 nm, respectively, and being from 20 nm to 100 nm in size wherein the nanoparticle spheres are prepared by:

(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 organic 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.

7. The oxide of titanium as defined in claim 6 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.

8. The oxide of titanium as defined in claim 7 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.

Assignments (7)
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 →
SECURITY INTEREST Recorded Mar 12, 2021
From: TRONOX LLC
To: HSBC BANK USA, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 055579/0619 →
SECURITY INTEREST Recorded May 1, 2020
From: TRONOX LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 052554/0529 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 10, 2019
From: CRISTAL USA INC.
To: TRONOX LLC
Reel/Frame 049148/0729 →
CHANGE OF NAME Recorded Jun 18, 2013
From: MILLENNIUM INORGANIC CHEMICALS, INC.
To: CRISTAL USA INC.
Reel/Frame 030650/0837 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 2, 2012
From: FU, GUOYI; WATSON, MARK
To: MILLENNIUM INORGANIC CHEMICALS, INC.
Reel/Frame 027639/0550 →