IP Library Granted Patent US 7,854,917
Granted Patent B2
US 7,854,917 · App. 12/067,091 · Granted Dec 21, 2010

Methods of controlling the particle size of titanium dioxide produced by the chloride process

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Quick Facts
Patent No.
US 7,854,917
App. No.
12/067,091
Granted
Dec 21, 2010
Kind
B2
Abstract

A process for manufacturing titanium dioxide by the chloride process is provided. In one embodiment, a particle size control agent comprising an ionizing agent such as potassium chloride is introduced into the reaction zone of the oxidation reactor to control the particle size of the titanium dioxide. In a first aspect, the effectiveness of the particle size control agent in controlling the particle size of the titanium dioxide is improved by adding the particle size control agent to at least one of the reactant streams at a sufficient distance upstream of the oxidization reactor to allow the ionizing agent to efficiently ionize and the particle size control agent to thoroughly admix with the stream(s) prior to entering the reaction zone. In a second aspect, the particle size control agent comprises an ionizing agent and fumed silica. In another embodiment, the amount of alumina added to the reaction zone of the oxidization reactor is increased in order to control the particle size of the titanium dioxide.

Claims (26)

1. A process for manufacturing titanium dioxide, comprising:

continuously reacting a titanium halide and an oxygen-containing gas in the vapor phase to produce titanium dioxide particles and gaseous reaction products, said reaction being carried out by combining a reactant stream of said titanium halide and a reactant stream of said oxygen-containing gas in a reaction zone of a vapor phase oxidation reactor at a temperature of at least 700° C.;

introducing a particle size control agent into said reaction zone to control the particle size of said titanium dioxide, said particle size control agent including an ionizing agent and fumed silica; and

separating said titanium dioxide particles from said gaseous reaction products.

2. The process of claim 1 , wherein said titanium halide is titanium tetrachloride.

3. The process of claim 1 , wherein said reaction is carried out at a pressure of at least about 15 psig.

4. The process of claim 3 , wherein said particle control agent is introduced to said reaction zone by adding said particle control agent to at least one of said reactant streams at a sufficient distance upstream of said oxidation reactor to allow said ionizing agent to efficiently ionize and said particle control agent in general to thoroughly admix with said stream(s) prior to entering said reaction zone.

5. The process of claim 1 , further comprising the step of introducing alumina to said reaction zone in a predetermined amount to promote rutilization of said titanium dioxide particles.

6. The process of claim 5 , further comprising controlling the particle size of said titanium dioxide by increasing the amount of alumina that is introduced to said reaction zone to an amount that is higher than said predetermined amount of alumina introduced to said reaction zone to promote rutilization of said titanium dioxide particles.

7. The process of claim 1 , wherein said ionizing agent is a metal ionizing agent.

8. The process of claim 7 , wherein said metal is selected from the group consisting of Groups IA and IIA and the Lanthanide Series of metals of the Periodic Table of the Elements.

9. The process of claim 1 , wherein said ionizing agent is potassium chloride.

10. The process of claim 1 , wherein said ionizing agent is a combination of potassium chloride and cesium chloride, the weight ratio of said potassium chloride and cesium chloride in said combination being in the range of from 100:1 to 100:9.

11. The process of claim 1 , wherein said particle size control agent further includes scour media.

12. The process of claim 1 , wherein the weight ratio of said ionizing agent to said fumed silica in said particle control agent is in the range of from about 3:1 to about 1:2.

13. The process of claim 12 , wherein the weight ratio of said metal ionizing agent to said fumed silica in said particle control agent is about 1:1.

14. The process of claim 1 , wherein said particle control agent is introduced to said reaction zone in an amount in the range of from about 100 parts to about 1,000 parts per million parts of said titanium dioxide particles being produced.

15. The process of claim 14 , further comprising the step of separately introducing an ionizing supplement directly to said reaction zone of said oxidation reactor.

16. The process of claim 15 , wherein ionizing supplement is introduced to said reaction zone in an amount in the range of from about 10 to about 3000 parts per million parts of said titanium dioxide particles being produced.

17. The process of claim 16 , wherein said ionizing supplement is introduced to said reaction zone of said oxidation reactor in at least two separate and discrete increments comprising a first increment and at least one additional increment, wherein said first increment is introduced to said reaction zone at a point therein prior to onset of reaction between said titanium halide and said oxygen-containing gas within said reaction zone, and wherein said at least one additional increment is introduced into said reaction zone at a point therein subsequent to the reaction of at least about 20 weight percent of said titanium halide with said oxygen-containing gas.

18. The process of claim 16 , wherein said ionizing supplement is potassium chloride.

19. A process for manufacturing titanium dioxide, comprising:

continuously reacting a titanium halide and an oxygen-containing gas in the vapor phase to produce titanium dioxide particles and gaseous reaction products, said reaction being carried out by combining a reactant stream of said titanium halide and a reactant stream of said oxygen-containing gas in a reaction zone of a vapor phase oxidation reactor at a temperature of at least 700° C. and a reaction pressure of at least about 15 psig;

introducing a particle size control agent into said reaction zone by addition to the titanium halide reactant stream, said particle size control agent including a metal ionizing agent and fumed silica, wherein said metal of said metal ionizing agent is selected from the group consisting of sodium, potassium, lithium, rubidium, cesium, calcium, barium, strontium, and cerium, and the weight ratio of said metal ionizing agent to said fumed silica in said particle size control agent is in the range of from about 3:1 to about 1:2, said particle size control agent being introduced to said reaction zone by adding said particle size control agent to at least one of said reactant streams at a sufficient distance upstream of said oxidation reactor to allow said metal ionizing agent to efficiently ionize and thoroughly admix with said stream(s) prior to entering said reaction zone; and

separating said titanium dioxide particles from said gaseous reaction products.

20. The process of claim 19 , wherein at least one of said titanium halide reactant stream and said oxygen-containing gas reactant stream is conducted to said oxidation reactor in a tubular conduit, and said particle size control agent is combined with said reactant stream in said tubular conduit at a point in said conduit that is a distance from the entrance to said oxidation reactor that is at least about 10 times the diameter of said conduit at the exit of said conduit.

Assignments (8)
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 →
SECURITY INTEREST Recorded Sep 25, 2017
From: TRONOX LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION
Reel/Frame 043993/0340 →
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 →