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Fluidized Coke-bed Chlorination of Ilmenites.
Harris-HM; Henderson-AW; Campbell-TT
NTIS: PB 258 104 :19 pages
The Bureau of Mines investigated chlorination of domestic ilmenites in a fluidized coke bed at temperatures of 950 deg to 1,150 deg c. Objectives were to develop an effective process for producing ticl4 suitable for tio2 pigment and to reduce pollution by collecting and treating waste byproduct chlorides. The reactor for these tests was a 10.2-Cm-diam quartz tube heated externally by electrical resistance heaters. It contained coke beds of from 35.6 to 82.5 Cm in depth that were fluidized by 13 to 25 l/min of chlorine. Ilmenite concentrate powders were introduced at the bottom of the fluid-bed reactor, using the chlorine gas stream as a carrier. Test results showed that greater than 90 pct of the ilmenite reacted at optimum conditions and recovery of ticl4 ranged from 95 to 99 pct of stoichiometric. A temperature-controlled cyclone was used to remove high-boiling-point chlorides such as mncl2, mgcl2, and fecl2, and also collected fine unreacted ilmenite and coke dust. Impure ticl4 and fecl3 were separated by collecting the iron chloride in a condenser controlled at 200 deg c. Titanium tetrachloride vapor was cleaned by passage through a salt-column filter followed by condensation in water-cooled and refrigerated condensers. Liquid ticl4 was purified further by well-known industrial methods to meet specifications for pigment-grade chloride. Integrated tests were conducted in which chlorine, produced by dechlorination of fecl3 with oxygen, was recycled and used directly in a fluidized-bed chlorinator.
IH; Report of Investigation;
NTIS Accession No.
NTIS: PB 258 104