PURIFICATION OF TiCl4 THROUGH THE PRODUCTION OF NEW CO-PRODUCTS
The present disclosure relates to reacting tin metal or SnCl 2 with crude TiCl 4 containing vanadium to produce pure TiCl 4 , SnCl 4 , and a vanadium solid co-product. 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 vanadium-containing crude TiCl 4 with tin to produce purified TiCl 4 , SnCl 4 , and solid vanadium; and
(b) separating the solid vanadium from the purified TiCl 4 and SnCl 4 .
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 1 , wherein the contacting and separating steps are performed by a two stage process comprising:
(i) reducing the vanadium content in the vanadium-containing crude TiCl 4 by contacting the vanadium-containing crude TiCl 4 with a less than excess amount of tin to produce partially purified TiCl 4 , SnCl 4 , and solid vanadium;
(ii) separating the solid vanadium from the partially purified TiCl 4 and SnCl 4 ;
(iii) further reducing the 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 vanadium, and excess tin; and
(iv) separating the solid vanadium 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 136° 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 vanadium 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 vanadium and excess tin of step (iv) back into the vanadium-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 vanadium-containing crude TiCl 4 with SnCl 2 to produce purified TiCl 4 , SnCl 4 , and solid vanadium; and
(b) separating 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 vanadium content in the vanadium-containing crude TiCl 4 by contacting the vanadium-containing crude TiCl 4 with a less than excess amount of SnCl 2 to produce partially purified TiCl 4 , SnCl 4 , and solid vanadium;
(ii) separating the solid vanadium from the partially purified TiCl 4 and SnCl 4 ;
(iii) further reducing the vanadium content in the partially purified TiCl 4 by contacting the partially purified TiCl 4 with an excess of SnCl 2 to produce purified TiCl 4 , SnCl 4 , solid vanadium, and excess SnCl 2 ; and
(iv) separating the solid vanadium and excess SnCl 2 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 136° 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 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 vanadium and excess SnCl 2 of step (iv) back into the vanadium-containing crude TiCl 4 of step (i); and
(vi) repeating steps (i)-(iv).