IP Library Granted Patent US 7,238,231
Granted Patent B1
US 7,238,231 · App. 11/600,643 · Granted Jul 3, 2007

Process for manufacturing zirconia-treated titanium dioxide pigments

Assignee: Tronox LLC
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Quick Facts
Patent No.
US 7,238,231
App. No.
11/600,643
Filed
Nov 16, 2006
Granted
Jul 3, 2007
Kind
B1
Art Unit
1755
USPC
106/417
Abstract

An improved process is described for manufacturing zirconia-treated titanium dioxide pigments, wherein the zirconia treatment is accomplished in the process of fluidizing a titanium dioxide filter or press cake and then drying the same, through the addition to the filter or press cake of one or more alkaline water-soluble zirconium reagents selected from ammonium zirconyl carbonate, the water-soluble ammonium zirconyl carboxylates and mixtures of these. Aqueous solutions of such zirconium reagents, in addition to being effective for imparting a zirconia surface treatment to the titanium dioxide materials, also prove to be effective fluidizing agents for forming high solids dispersions of the zirconia-treated titanium dioxide pigment materials which can be spray dried without substantial dilution and excessive energy requirements.

Claims (19)

1. A process for manufacturing zirconia-treated titanium dioxide, comprising the steps of:

a) forming a mixture comprising a titanium dioxide material in water;

b) wet milling said mixture;

c) after step b), optionally depositing on said wet milled titanium dioxide material one or more inorganic oxides selected from the group consisting of the oxides of aluminum, boron, cerium, phosphorus, silicon, tin, titanium and zirconium;

d) achieving a pH of the mixture resulting from steps b) or c) between about 5 and about 9, whereby the titanium dioxide material is sufficiently flocculated to be recovered by vacuum or pressure filtration;

e) removing said titanium dioxide material from said mixture by vacuum or pressure filtration;

f) washing the titanium dioxide material recovered by filtration;

g) converting the washed titanium dioxide material to a fluid dispersion by addition of one or more alkaline water-soluble zirconium reagents selected from the group consisting of ammonium zirconyl carbonate, the water-soluble ammonium zirconyl carboxylates and mixtures of these;

h) drying the dispersion to yield a dry zirconia surface treated titanium dioxide powder.

2. A process as defined in claim 1 , wherein the titanium dioxide material is a rutile titanium dioxide intermediate produced from titanium tetrachloride using a vapor phase oxidation step.

3. A process as defined in claim 2 , wherein the titanium dioxide material acted upon possesses a crystalline lattice, and is further characterized in that, other than any inorganic oxides formed in the crystalline lattice of the titanium dioxide intermediate during the vapor phase oxidation step, substantially no inorganic oxides have been deposited on said titanium dioxide material prior to optional step c) or step g).

4. A process as defined in claim 1 , wherein after the addition of one or more alkaline water-soluble zirconium reagents, the resulting fluid dispersion is characterized by a titanium dioxide solids content of at least about 50 percent by weight.

5. A process as defined in claim 4 , wherein the resulting fluid dispersion is characterized by a titanium dioxide solids content of at least about 55 percent by weight.

6. A process as defined in claim 5 , wherein the resulting fluid dispersion is characterized by a titanium dioxide solids content of at least about 60 percent by weight.

7. A process as defined in claim 1 , wherein the one or more alkaline water-soluble zirconium reagents are selected from the group consisting of ammonium zirconyl carbonate, ammonium zirconyl acetate, ammonium zirconyl formate and mixtures thereof.

8. A process as defined in claim 1 , wherein the one or more alkaline water-soluble zirconium reagents are added in aqueous solution form, in which the zirconium reagent or reagents are present at a concentration of between about 20 percent and about 50 percent.

9. A process as defined in claim 1 , wherein the water-soluble zirconium reagents used represents between about 0.05 percent and 1.5 percent by weight of finished pigment of deposited zirconia.

10. A process as defined in claim 1 , wherein the water-soluble zirconium reagents used represents between about 0.1 percent and 0.5 percent by weight of finished pigment of deposited zirconia.

11. A process as defined in claim 1 , wherein the drying step is performed by spray drying of the dispersion.

Assignments (18)
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 →
ASSIGNMENT OF SECURITY INTEREST IN PATENT COLLATERAL RECORDED AT REEL/FRAME 044100/0339 Recorded Mar 12, 2021
From: BANK OF AMERICA, N.A.
To: HSBC BANK USA, NATIONAL ASSOCIATION, AS THE SUCCESSOR ADMINISTRATIVE AGENT AND COLLATERAL AGENT
Reel/Frame 055578/0880 →
RELEASE OF SECURITY INTEREST Recorded Mar 12, 2021
From: WELLS FARGO BANK, NATIONAL ASSOCIATION
To: TRONOX LLC
Reel/Frame 055583/0001 →
SECURITY INTEREST Recorded May 1, 2020
From: TRONOX LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 052554/0529 →
PATENT SECURITY AGREEMENT Recorded Oct 2, 2017
From: TRONOX LLC
To: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
Reel/Frame 044100/0339 →
RELEASE OF SECURITY INTEREST IN INTELLECTUAL PROPERTY COLLATERAL AT REEL/FRAME NOS. 027682/0086 AND 030047/0422 Recorded Sep 26, 2017
From: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
To: TRONOX LLC
Reel/Frame 044018/0893 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Sep 25, 2017
From: UBS AG, STAMFORD BRANCH, AS COLLATERAL AGENT
To: TRONOX LLC; TRONOX WORLDWIDE LLC
Reel/Frame 043993/0306 →
SECURITY INTEREST Recorded Sep 25, 2017
From: TRONOX LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION
Reel/Frame 043993/0340 →
PATENT SECURITY AGREEMENT Recorded Jul 18, 2012
From: TRONOX LLC; TRONOX WORLDWIDE LLC
To: UBS AG, STAMFORD BRANCH
Reel/Frame 028582/0669 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 12, 2012
From: WELLS FARGO CAPITAL FINANCE, LLC
To: TRONOX LLC; TRONOX WORLDWIDE LLC
Reel/Frame 028535/0362 →
SECURITY AGREEMENT Recorded Feb 9, 2012
From: TRONOX LLC
To: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
Reel/Frame 027682/0086 →
RELEASE OF SECURITY INTEREST Recorded Feb 9, 2012
From: GOLDMAN SACHS LENDING PARTNERS LLC
To: TRONOX LLC
Reel/Frame 027682/0064 →
BANKRUPTCY COURT NOTICE CONFIRMING RELEASE OF LIENS EFFECTIVE 2/14/2011 Recorded Mar 24, 2011
From: LEHMAN COMMERCIAL PAPER, INC.
To: TRONOX LLC
Reel/Frame 026010/0684 →
SECURITY AGREEMENT Recorded Feb 22, 2011
From: TRONOX LLC; TRONOX PIGMENTS (SAVANNAH) INC.
To: WELLS FARGO CAPITAL FINANCE, LLC, AS AGENT
Reel/Frame 025822/0026 →
SECURITY AGREEMENT Recorded Feb 15, 2011
From: TRONOX LLC
To: GOLDMAN SACHS LENDING PARTNERS LLC, AS COLLATERAL AGENT
Reel/Frame 025795/0130 →
SECURITY AGREEMENT Recorded Aug 21, 2008
From: TRONOX LLC F/K/A KERR-MCGEE CHEMICAL LLC
To: LEHMAN COMMERCIAL PAPER INC.
Reel/Frame 021411/0792 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 16, 2006
From: CRAIG, DANIEL H.; ELLIOTT, JEFFREY D.; RAY, HARMON E.
To: TRONOX LLC
Reel/Frame 018612/0545 →