Process for producing titanium dioxide particles having reduced chlorides
View Patent ↗This disclosure relates to process for producing titanium dioxide pigment having reduced chlorides, comprising: a) reacting titanium tetrahalide vapor, rutile-forming agent and at least a stoichiometric amount of oxygen in a reactor to form a gaseous suspension comprising titanium dioxide particles; b) introducing silicon tetrachloride into the reactor at least one point downstream of the point of contact of the titanium tetrahalide, the rutile forming agent and the oxygen, and where at least 97% of the titanium tetrahalide has been converted to titanium dioxide to provide a substantially uniform encapsulation of pyrogenic SiO 2 on the titanium dioxide; c) passing the gaseous suspension to a cooling conduit; d) introducing scouring material, typically selected from the group of calcined titanium dioxide and compressed titanium dioxide, and mixtures thereof, into the cooling conduit; wherein the particles of the scouring material have a diameter in the range of about 0.25 mm to about 12.7 mm and forming a cooled product having a solid and a vapor phase; e) separating the vapor phase from the cooled product to form a powder comprising the titanium dioxide particles, and a content of chlorine-containing material ranging from about 500 to about 3000 ppm of oxychloride, and the scouring material; and f) subjecting the powder to substantially uniform heating at a temperature of about 200° C. to about 600° C., in the presence of moisture, to reduce the content of chlorine-containing material to less than about 60 ppm oxychloride; wherein the moisture present is in at least a stoichiometric amount with the oxychloride.
1. A process for producing titanium dioxide pigment, comprising:
a) reacting titanium tetrahalide vapor, a rutile-forming agent and at least a stoichiometric amount of oxygen in a reactor to form a gaseous suspension comprising titanium dioxide particles;
b) introducing silicon tetrachloride into the reactor at least one point downstream of the point of contact of the titanium tetrahalide, the rutile forming agent and the oxygen, and where at least 97% of the titanium tetrahalide has been converted to titanium dioxide;
c) passing the gaseous suspension to a cooling conduit;
d) introducing scouring, material particles, selected from the group consisting of calcined titanium dioxide and compressed titanium dioxide, and mixtures thereof, into the cooling conduit; wherein the scouring material particles have a diameter in the range of about 0.25 mm to about 12.7 mm and forming a cooled product having a solid and a vapor phase;
e) separating the vapor phase from the cooled product to form a powder comprising the titanium dioxide particles, chlorine-containing material comprising about 500 to about 3000 ppm of one or more oxychlorides, and the scouring material; and
f) subjecting the powder to fluid energy milling in a fluid energy mill and substantially uniform heating at a temperature of about 200° C. to about 600° C., in the presence of moisture, the substantially uniform heating in the presence of moisture taking place in the fluid energy mill, to reduce the content of chlorine containing materials to an oxychlorides content of less than about 60 ppm; wherein the moisture present is in at least a stoichiometric amount with the oxychloride.
2. The process of claim 1 wherein the chlorine-containing material comprises about 30 to about 40 ppm of one or more oxychlorides.
3. The process of claim 1 wherein: step (f) forms a milled powder comprising particles having a mean particle size of about 50 nm to about 1000 nm.
4. The process of claim 3 wherein step (f) forms a milled powder comprising particles having a mean particle size of about 100 nm to about 250 nm.
5. The process of claim 1 wherein the temperature is about 250° C. to about 400° C.
6. The process of claim 3 wherein the fluid energy mill comprises a heated fluid selected from the group consisting of steam, aft, argon, helium, nitrogen and mixtures thereof.
7. The process of claim 6 where in the heated fluid is steam.
8. The process of claim 1 wherein the fluid energy mill is a micronizer.
9. The process of claim 8 wherein the micronizer comprises a heated fluid selected from the group consisting of steam, air, argon, helium, nitrogen and mixtures thereof.
10. The process of claim 9 wherein the heated fluid is steam.
11. The process of claim 8 wherein the powder is substantially uniformly heated at a temperature of about 250° C. to about 400° C.
12. The process of claim 11 wherein the powder is substantially uniformly heated at a temperature of about 250° C. to about 300° C.
13. The process of claim 1 wherein step (f) is carried out in a space having a vapor space the vapor space having an amount of free chlorine and the amount of free chlorine in the vapor space is less than about 1 ppm.
14. The process of claim 1 wherein the rutile-forming argent aluminum halide.