RI 8165 Fluidized Coke-Bed Chlorination of Ilmenites

The Bureau of Mines investigated chlorination of domestic ilmenites in a fluidized coke bed at temperatures of 950° to 1,150° C. Objectives were to develop an effective process for producing TiC14 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 TiC14 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 TiC14 and FeC13 were separated by collecting the, iron chloride in a condenser con-trolled at 200° C. Titanium tetrachloride vapor was cleaned by passage-through a salt-column filter followed by condensation in water-cooled and refrigerated condensers. Liquid TiC14 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 FeC13 with oxygen, was recycled and used directly in a fluidized-bed chlorinator.