Liquid titanium chloride

Example 7

First, 120 g of a titanium-aluminum-vanadium chloride mixture was prepared, by mixing liquid titanium chloride (from Sigma Aldrich), aluminum chloride powder (from Strem Chemical) and liquid vanadium chloride (from Acros Organics). The mixture was stirred constantly to maintain a dispersion of the aluminum chloride.

Next, 140 g of sodium metal was heated to 250° C. in an Inconel vessel and stirred by a Cowles blade mixer at speeds ranging from 1000 rpm initially, to 2500 rpm as the reaction progressed. The chloride mixture was pumped into the reactor until 74 g had been added, over approximately 90 minutes. The reaction stopped when the vortex in the sodium could no longer be maintained.

The reactor vessel was then sealed and transferred to a furnace, brought to 825° C. and held at that temperature for approximately one hour before being allowed to cool.

The recovered product was then washed to remove the sodium chloride coating the metal powder, and the powder was dried in a vacuum oven at 100 C for 24 hours.

Analysis of the metal powder using ICPMS showed the product contained under 50 ppm iron and under 150 ppm total transition metals. The results demonstrate that the titanium powder falls within the purity limits as described in UNS No. R56400.

Example 7

First, 120 g of a titanium-aluminum-vanadium chloride mixture was prepared, by mixing liquid titanium chloride (from Sigma Aldrich), aluminum chloride powder (from Strem Chemical) and liquid vanadium chloride (from Acros Organics). The mixture was stirred constantly to maintain a dispersion of the aluminum chloride.

Next, 140 g of sodium metal was heated to 250° C. in an Inconel vessel and stirred by a Cowles blade mixer at speeds ranging from 1000 rpm initially, to 2500 rpm as the reaction progressed. The chloride mixture was pumped into the reactor until 74 g had been added, over approximately 90 minutes. The reaction stopped when the vortex in the sodium could no longer be maintained.

The reactor vessel was then sealed and transferred to a furnace, brought to 825° C. and held at that temperature for approximately one hour before being allowed to cool.

The recovered product was then washed to remove the sodium chloride coating the metal powder, and the powder was dried in a vacuum oven at 100 C for 24 hours.

Analysis of the metal powder using ICPMS showed the product contained under 50 ppm iron and under 150 ppm total transition metals. The results demonstrate that the titanium powder falls within the purity limits as described in UNS No. R56400.

Example 7

First, 120 g of a titanium-aluminium-vanadium chloride mixture was prepared, by mixing liquid titanium chloride (from Sigma Aldrich), aluminium chloride powder (from Strem Chemical) and liquid vanadium chloride (from Acros Organics). The mixture was stirred constantly to maintain a dispersion of the aluminum chloride.

Next, 140 g of sodium metal was heated to 250° C. in an inconel vessel and stirred by a Cowles blade mixer at speeds ranging from 1000 rpm initially, to 2500 rpm as the reaction progressed. The chloride mixture was pumped into the reactor until 74 g had been added, over approximately 90 minutes. The reaction stopped when the vortex in the sodium could no longer be maintained.

The reactor vessel was then sealed and transferred to a furnace, brought to 825° C. and held at that temperature for approximately one hour before being allowed to cool.

The recovered product was then washed to remove the sodium chloride coating the metal powder, and the powder was dried in a vacuum oven at 100 C for 24 hours.

Analysis of the metal powder using ICPMS showed the product contained under 50 ppm iron and under 150 ppm total transition metals. The results demonstrate that the titanium powder falls within the purity limits as described in UNS No. R56400.