Purification of TiCl
View Patent ↗The present disclosure relates to reacting tin metal with crude TiCl 4 containing arsenic to produce pure TiCl 4 , SnCl 4 , and an arsenic solid co-product. In some embodiments, the contaminant vanadium is removed as well. In another embodiment, the vanadium is removed separately through a commercial process and the resulting arsenic containing commercial grade of purified TiCl 4 is reacted with elemental tin, sulfur and ferric chloride to substantially reduce the arsenic. The reaction is preferably done in a continuous fashion in two stages for maximum through-put and utility at an elevated temperature. Distillation can be used to purify the TiCl 4 produced and simultaneously yield a purified SnCl 4 product. The synthesis of SnCl 4 in this method utilizes waste chloride to save virgin chlorine which would otherwise be used.
1. A process for arsenic purification of a commercial purified TiCl 4 comprising:
(i) contacting an arsenic-containing commercial purified TiCl 4 substantially free of vanadium with elemental sulfur, ferric chloride, and elemental tin; and
(ii) producing purified TiCl 4 , SnCl 4 , and solid arsenic.
2. The process of claim 1 further comprising:
(iii) separating the purified TiCl 4 from the SnCl 4 .
3. The process of claim 2 , wherein the step of separating the purified TiCl 4 from the SnCl 4 is performed by distillation.
4. The process of claim 1 , wherein step (i) is performed at a temperature of at least 100° C.
5. The process of claim 1 , wherein step (i) is performed at a temperature in the range of at least about 150° C. to at least about 200° C.