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. 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 the purification of TiCl 4 comprising:
(a) contacting arsenic-containing crude TiCl 4 with tin; and
(b) producing purified TiCl 4 , SnCl 4 , and solid arsenic.
2. The process of claim 1 comprising after step (b) the further step of 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 2 , further comprising:
(i) reducing the arsenic content in the arsenic-containing crude TiCl 4 by contacting the arsenic-containing crude TiCl 4 with a less than excess amount of tin to produce partially purified TiCl 4 , SnCl 4 , and solid arsenic;
(ii) separating the solid arsenic from the partially purified TiCl 4 and SnCl 4 ;
(iii) further reducing the arsenic content in the partially purified TiCl 4 by contacting the partially purified TiCl 4 with an excess of tin to produce purified TiCl 4 , SnCl 4 , solid arsenic, and excess tin; and
(iv) separating the solid arsenic and excess tin from the purified TiCl 4 and SnCl 4 .
5. The process of claim 4 , wherein step (i) is performed at a temperature of at least 100° C.
6. The process of claim 5 , wherein step (i) is performed at a temperature in the range of at least about 150° C. to at least about 200° C.
7. The process of claim 4 , wherein the solid arsenic of step (iv) is substantially free of residual treating agents.
8. The process of claim 4 comprising after step (iv) the further steps of:
(v) recycling the solid arsenic and excess tin of step (iv) back into the arsenic-containing crude TiCl 4 of step (i); and
(vi) repeating steps (i)-(iv).
9. A process for the purification of TiCl 4 comprising:
(a) contacting arsenic- and vanadium-containing crude TiCl 4 with tin to produce purified TiCl 4 , SnCl 4 , solid arsenic, and solid vanadium; and
(b) separating the solid arsenic and the solid vanadium from the purified TiCl 4 and SnCl 4 .
10. The process of claim 9 comprising after step (b) the further step of separating the purified TiCl 4 from the SnCl 4 .
11. The process of claim 10 , wherein the step of separating the purified TiCl 4 from the SnCl 4 is performed by distillation.
12. The process of claim 9 , wherein the contacting and separating steps are performed by a two stage process comprising:
(i) reducing the arsenic and vanadium content in the arsenic- and vanadium-containing crude TiCl 4 by contacting the arsenic- and vanadium-containing crude TiCl 4 with a less than excess amount of tin to produce partially purified TiCl 4 , SnCl 4 , solid arsenic, and solid vanadium;
(ii) separating the solid arsenic and the solid vanadium from the partially purified TiCl 4 and SnCl 4 ;
(iii) further reducing the arsenic and vanadium content in the partially purified TiCl 4 by contacting the partially purified TiCl 4 with an excess of tin to produce purified TiCl 4 , SnCl 4 , solid arsenic, solid vanadium, and excess tin; and
(iv) separating the solid arsenic and the solid vanadium and excess tin from the purified TiCl 4 and SnCl 4 .
13. The process of claim 12 , wherein step (i) is performed at a temperature of at least 100° C.
14. The process of claim 13 , wherein step (i) is performed at a temperature in the range of at least about 150° C. to at least about 200° C.
15. The process of claim 12 , wherein the solid arsenic and the solid vanadium of step (iv) is substantially free of residual treating agents.
16. The process of claim 12 comprising after step (iv) the further steps of:
(v) recycling the solid arsenic, the solid vanadium, and excess tin of step
(iv) back into the arsenic- and vanadium-containing crude TiCl 4 of step (i); and
(vi) repeating steps (i)-(iv).