摘要 |
<p>1,213,089. Purifying titanium tetrachloride; sulphur. MONTECATINI EDISON S.p.A. 12 May, 1969 [10 May, 1968], No. 24036/69. Heading C1A. Vanadium compounds (e.g. VOCl 3 , VCl 4 ) which exist as impurities in titanium tetrachloride are removed therefrom by treating with hydrogen sulphide at from 130-180‹ C., the amount of hydrogen sulphide used being from 1 to 3 mols. per mol. of vanadium compound present, whilst at the same time cooling the crude titanium tetrachloride by injection of liquid titanium tetrachloride. The process may be carried out in a spray-quencher, and the contact time (for the reaction) should be at least 10 seconds, preferably 15-50 seconds. Afterwards the vapours may be scrubbed with liquid titanium tetrachloride, this liquid being recycled to the hydrogen sulphide treatment and the gaseous purified titanium tetrachloride sent for rectification. The gases may be passed through a cyclone between the spray-quencher and scrubbing apparatus to remove some of the solid particles, some of which collect in the sprayquencher. The process may be used to treat impure titanium tetrachloride made by chlorinating titaniferous material. Molten elementary sulphur formed in the reaction between hydrogen sulphide and the vanadium compounds is discharged with solid impurities from the spray-quencher and cyclone. In Example 1, the solids contained 4.9% sulphur and in Example 2, where a larger ratio of H 2 5 was used per mol. of vanadium compounds the solids contained about 25% by weight of sulphur.</p> |