Conversion of compounds of titanium in a plus 4 oxidation state to titanium compounds in a plus 3 oxidation state

The method which comprises:

• (i) providing a reactor containing a titanium tetrahalide, and particulate titanium, and
• (ii) adding an ether which forms a complex with titanium trihalide to the contents of said reactor,
• wherein a reaction mixture containing a complex of a titanium trihalide and said ether is produced, and
• wherein said complex is insoluble in said reaction mixture.

The method for preparing a complex of a titanium trihalide and an ether which comprises:

• (i) providing a mixture of a titanium tetrahalide, particulate titanium, and a non-interfering medium in a reactor,
• (ii) adding an ether which forms a complex with titanium trihalide to said step (i) mixture in said reactor
• wherein an exothermic reaction occurs and a first reaction mixture is produced, and
• wherein the pot temperature in said reactor is maintained between about 10° C. and about 20° C. during said addition of said ether to said mixture in said reactor, and
• (iii) thereafter raising the temperature of said first reaction mixture in said reactor to about 90° C. to 100° C., and
• (iv) refluxing said first reaction mixture in said reactor at about 90° C. to 100° C.
• wherein a second reaction mixture containing an adduct of said ether and a titanium trihalide is produced in said reactor.

A method which comprises:

• (i) providing a mixture of TiCl4, particulate titanium metal and toluene in a chilled reactor,
• (ii) adding tetrahydrofuran or dimethoxyethane to said step (i) mixture in said reactor wherein an exothermic reaction occurs,
• (iii) maintaining the pot temperature of said reactor at about 10° C. to 30° C. for the substantial duration of said exothermic reaction and thereafter raising said pot temperature to reflux temperature,
• (iv) refluxing said first reaction mixture for at least about four hours
• wherein a second reaction mixture comprising a TiCl3.tetrahydrofuran complex or a TiCl3.dimethoxyethane complex and toluene is produced, and
• (v) recovering said complex from said step (iv) second reaction mixture.

A method which consists essentially of

• (i) treating titanium tetrachloride with particulate titanium in the presence of an ether which forms an adduct with titanium trichloride
• wherein a reaction mixture containing a complex of titanium trichloride and said ether is produced, and
• wherein said treating is conducted in a medium in which said adduct is insoluble;
• (ii) separating said adduct from said reaction mixture;
• and
• (iii) washing and drying said separated adduct
• wherein a titanium trichloride ether adduct free of contamination with halides of metals other than titanium is produced.