| 摘要 |
1,193,371. Titanium halides. MIZUSAWA KAGAKU KOGYO K.K. 10 Jan., 1968 [10 Jan., 1967], No. 1491/68. Heading C1A. Titanium tetrahalides are prepared by forming mixture of a hydrogel or a xerogel of a titanium salt of a phosphorus oxyacid with at least one halide of an alkaline earth metal, heating the mixture in the solid phase under non- oxidizing conditions at a temperature between 300‹ C. and the highest temperature at which the mixture can remain in the solid state for a period of time sufficient to form the titanium halide, and thereafter recovering the halide produced. The said phosphorus oxyacid may be orthophosphoric, metaphosphoric, pyrophosphoric, hexametaphosphoric, tripolyphosphoric, phosphorous, or hypophosphorous acid, and the alkaline earth metal halide is preferably the chloride, bromide, or iodide, of Mg, Ca, Ba, or Sr, and may be a fluoride, but these tend to cause corrosion of the apparatus. Sufficient halide is used to provide 4 atoms of halogen per atom of Ti, and the halide and gel may be ground together as a paste using water, or the mixture formed by mixing a hydrosol of the Ti compound with the halide, in each case the resulting mixture being dried at a temperature not exceeding 400‹ C. The mixture is then heated in an atmosphere of argon, nitrogen, carbon dioxide, hydrogen, halogen, methane or a vacuum, and the product titanium halide is collected by cooling to a temperature between - 50‹ C. and room temperature. The titanium salt gel may be prepared as described in Specification 1,161,141. |
