IP Library Granted Patent US 7,344,591
Granted Patent B2
US 7,344,591 · App. 11/743,528 · Granted Mar 18, 2008

Stabilized suspension of titanium dioxide nanoparticles and methods of manufacture

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Quick Facts
Patent No.
US 7,344,591
App. No.
11/743,528
Granted
Mar 18, 2008
Kind
B2
Abstract

Titanium dioxide nanoparticles are formed using a dispersing agent to form nanoparticles with desired size, shape, and uniformity. The titanium dioxide nanoparticles are formed by reacting an inorganic titanium compound with water or ice to form an aqueous titanium compound. The aqueous titanium compound is reacted or combined with a dispersing agent. Titanium dioxide nanoparticles are precipitated to form a suspension. The formation of the titanium dioxide nanoparticles is influenced by the presence of bonding of the dispersing agent. The size of the nanoparticles can be advantageously controlled by selecting the ratio of titanium to dispersing agent. In addition, the titanium dioxide nanoparticles can be used in suspension form or filtered and dried to form a powder.

Claims (32)

1. A suspension of stabilized titanium dioxide nanoparticles, comprising:

a solvent substantially free of a monofunctional alcohol;

a dispersing agent comprising a plurality of organic molecules that have at least one functional group selected from the group consisting of a hydroxyl, a carboxyl, a carbonyl, an amide, an amine, a thiol, a sulfonic acid, sulfonyl halide, an acyl halide, and combinations thereof; and

a plurality of titanium dioxide nanoparticles dispersed in the solvent to form a suspension of nanoparticles stabilized by the dispersing agent,

wherein the titanium dioxide nanoparticles have a particle size of up to 200 nm.

2. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the organic molecules of the dispersing agent comprise at least two different functional groups selected from the group consisting of hydroxyl, carboxyl, carbonyl, amide, amine, thiol, sulfonic acid, sulfonyl halide.

3. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the dispersing agent comprises at least one type of organic molecules selected from the group consisting of glycolic acid, glycine, L-alanine, and β-alanine.

4. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the titanium dioxide nanoparticles have a particle size of up to 100 nm.

5. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the titanium dioxide nanoparticles have a particle size of up to about 20 nm.

6. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the titanium dioxide nanoparticles have a particle size of up to 4 nm.

7. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the suspension has a temperature less than about 10° C. so as to have increased stability over time.

8. A suspension of stabilized titanium dioxide nanoparticles as in claim 1 , wherein the suspension has a temperature less than about 0° C. so as to have increased stability over time.

9. A suspension of stabilized titanium dioxide nanoparticles, comprising:

a solvent;

a dispersing agent comprising a plurality of organic molecules selected from the group consisting of glycolic acid, glycine, L-alanine, and β-alanine; and

a plurality of titanium dioxide nanoparticles dispersed in the solvent to form a suspension of nanoparticles stabilized by the dispersing agent,

wherein the titanium dioxide nanoparticles have a particle size of up to 200 nm.

10. A suspension of stabilized titanium dioxide nanoparticles as in claim 9 , wherein the titanium dioxide nanoparticles have a particle size of up to 100 nm.

11. A suspension of stabilized titanium dioxide nanoparticles as in claim 9 , wherein the titanium dioxide nanoparticles have a particle size of up to about 20 nm.

12. A suspension of stabilized titanium dioxide nanoparticles as in claim 9 , wherein the suspension has a temperature less than about 10° C. so as to have increased stability over time.

13. A suspension of stabilized titanium dioxide nanoparticles as in claim 9 , wherein the suspension has a temperature less than about 0° C. so as to have increased stability over time.

14. A suspension of stabilized titanium dioxide nanoparticles of controlled particle size manufactured according to a method comprising:

(i) reacting an inorganic titanium compound with water to form an aqueous titanium solution;

(ii) adding an amount of a dispersing agent to the aqueous titanium solution to form a precursor solution, wherein the dispersing agent comprises plurality of organic molecules that have at least one functional group capable binding to titanium in the aqueous solution;

(iii) forming a suspension of titanium dioxide nanoparticles having a particle size up to 200 nm by holding the precursor solution at one or more temperatures in a range of about 15° C. to about 155° C. until form out the precursor solution in the presence of the dispersing agent; and

(iv) cooling the suspension of titanium dioxide nanoparticles to a temperature below the one or more temperatures to yield a suspension of stabilized titanium dioxide nanoparticles of controlled particle size, the dispersing agent further stabilizing the titanium dioxide nanoparticles.

15. A suspension of stabilized titanium dioxide nanoparticles as in claim 14 , wherein the at least one functional group is selected from the group consisting of a hydroxyl, a carboxyl, a carbonyl, an amide, an amine, halide, an acyl halide, and combinations thereof.

16. A suspension of stabilized titanium dioxide nanoparticles as in claim 14 , wherein the dispersing agent comprises at least one type of organic molecules selected from the group consisting of glycolic acid, glycine, L-alanine, and β-alanine.

17. A suspension of stabilized titanium dioxide nanoparticles as in claim 14 , wherein the inorganic titanium compound is reacted in (i) with water at about 0° C. and/or with ice.

18. A suspension of stabilized titanium dioxide nanoparticles as in claim 14 , wherein the suspension of titanium dioxide nanoparticles is cooled in (iv) to a temperature less about 10° C.

19. A suspension of stabilized titanium dioxide nanoparticles as in claim 14 , wherein the suspension of titanium dioxide nanoparticles is cooled in (iv) to a temperature less about 0° C.

20. A suspension of stabilized titanium dioxide nanoparticles as in claim 14 , wherein the dispersing agent is added to the titanium solution in (ii) in a ratio of titanium atoms to functional groups of about 0.01 to about 100 so that that titanium dioxide nanoparticles are formed in (iii) having a size between about 2 nm and 200 nm.

Assignments (7)
RELEASE OF SECURITY INTEREST Recorded May 8, 2017
From: DEUTSCHE BANK AG NEW YORK BRANCH
To: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.; HEADWATERS HEAVY OIL, LLC
Reel/Frame 042422/0740 →
SECURITY AGREEMENT Recorded Sep 17, 2015
From: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.
To: DEUTSCHE BANK AG NEW YORK BRANCH, AS ADMINISTRATIVE AGENT
Reel/Frame 036628/0277 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 22, 2015
From: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.
To: HEADWATERS TECHNOLOGY INNOVATION, LLC
Reel/Frame 035473/0518 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 22, 2015
From: HEADWATERS TECHNOLOGY INNOVATION, LLC
To: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.
Reel/Frame 035473/0576 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 22, 2015
From: HEADWATERS NANOKINETIX, INC.
To: HEADWATERS TECHNOLOGY INNOVATION GROUP, INC.
Reel/Frame 035473/0429 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 22, 2015
From: ZHOU, BING; PARASHER, SUKESH; WU, ZHIHUA; ZHOU, ZHENHUA
To: HEADWATERS NANOKINETIX, INC.
Reel/Frame 035473/0311 →
PATENT RELEASE (REEL:23699/FRAME:0452) Recorded Mar 26, 2015
From: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: HEADWATERS INCORPORATED, AS GRANTOR; HEADWATERS RESOURCES, INC., A UTAH CORPORATION; HEADWATERS TECHNOLOGY INNOVATION GROUP, INC., A UTAH CORPORATION; HEADWATERS HEAVY OIL, LLC, A UTAH CORPORATION; TAPCO INTERNATIONAL CORPORATION, A MICHIGAN CORPORATION
Reel/Frame 035306/0558 →