12037-65-9

hard, gray metallic powder(s) with hexagonal structure; prepared by heating phosphine with TiCl4; stable up to 1400°C; finds use as a catalyst in organic reactions [KIR83]

2 g of Ti filings ground to pinhead size and 4 g of red P are weighed into a small ceramic or sintered clay cylindrical crucible. The materials are degassed by fanning with a high vacuum flame and then sealed (in vacuum) into a quartz pressure tube. The colder half of the tube is heated to 450 °C, while the Ti side is maintained at 950 °C. Two three-day periods are needed for the reaction. After the first period, the tube is slowly cooled for 3-4 hours, and the unreacted P is thus distilled into the cooler section. The grinding is carried out under CSS, which is then removed with alcohol and dried in a vacuum over NaOH at 120-140 ℃. Microscopic examination of the dark-gray metallic product should show no red phosphorus. The phosphorus quantity used for the second reaction stage should again correspond to an atomic ratio of 3 P: 1 Ti. The product treatment after the second three-day heating period is the same as after the first. The resultant phosphide does not correspond entirely to the formula TiP (maximum composition is TiP0 . 9 3 ).