Method for carrying out vanadium removal on coarse titanium tetrachloride
A technology of coarse titanium tetrachloride and titanium tetrachloride, which is applied in the direction of titanium tetrachloride and titanium halide, can solve the problems of aluminum trichloride not up to standard and mildness, and achieve less residue, good settling performance, and Good effect of vanadium
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[0029] According to a preferred embodiment of the present invention, the step of removing vanadium from the aluminum powder includes: preparing a titanium trichloride slurry, and performing a second contact with the liquid phase obtained in step (1) with the titanium trichloride slurry.
[0030] Wherein, the preparation process of the titanium trichloride slurry can be a conventional choice in the art, for example, the titanium trichloride slurry can be prepared with aluminum powder and titanium tetrachloride in the presence of aluminum trichloride, or it can be prepared in the general Prepare titanium trichloride slurry with aluminum powder and titanium tetrachloride under the condition of chlorine gas.
[0031] According to a preferred embodiment of the present invention, the present invention uses aluminum powder and titanium tetrachloride to prepare titanium trichloride slurry under the condition of flowing chlorine gas. Specifically, under an inert atmosphere, mix refined...
Embodiment 1
[0042] This embodiment is used to illustrate the method that the crude titanium tetrachloride provided by the present invention removes vanadium
[0043] (1) 500 g of crude titanium tetrachloride having a vanadium content of 0.5% by weight and 15 g of mineral oil were added to a round bottom flask, and stirred at 45° C. for 1 hour. There is no phenomenon of residue sticking to the wall. The mixture in the round-bottomed flask was placed in a 1L measuring cylinder, and was left to settle at 25° C. for 3 hours to obtain 419 g of liquid phase and 94 g of vanadium-containing mud in the lower layer. Then samples were taken at different heights of the liquid phase, and the solid content and vanadium content (measured by taking the supernatant after centrifugation) were carried out by centrifugation. Among them, the maximum solid content of the liquid phase part is 9g / L. After analysis, the vanadium content in the liquid phase was 0.1336% by weight.
[0044] (2) Under the protecti...
Embodiment 2
[0047] This embodiment is used to illustrate the method that the crude titanium tetrachloride provided by the present invention removes vanadium
[0048] (1) 500 g of crude titanium tetrachloride having a vanadium content of 0.5% by weight, 2.5 g of nonanoic acid, and 2.5 g of oleic acid were added to a round bottom flask, and stirred at 80° C. for 0.5 hours. There is no phenomenon of residue sticking to the wall. The mixture in the round-bottomed flask was placed in a 1L measuring cylinder, and was left to settle at 30° C. for 1 hour to obtain 404 g of liquid phase and 97 g of vanadium-containing mud in the lower layer. Then samples were taken at different heights of the liquid phase, and the solid content and vanadium content were determined by centrifugation. Wherein, the maximum solid content of the liquid phase part is 10g / L. After analysis, the vanadium content in the liquid phase was 0.1109% by weight.
[0049] (2) Under the protection of nitrogen, prepare a suspensi...
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